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  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Cellular and molecular life sciences 42 (1986), S. 448-450 
    ISSN: 1420-9071
    Keywords: Lepidoptera ; Acrolepiopsis assectella ; host plant ; larval diet ; ovarian production ; stimulation ; insemination
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Notes: Summary Females ofAcrolepiopsis assectella, reared on a semi-synthetic diet and laying on artificial substrates, do not respond to external stimuli by increasing ovarian production. When returned to the natural host (Allium porrum) for only one generation, ovarian production again rises and reaches the same level as in wild females, but its variability is strongly reduced. We conclude that selection under artificial conditions eliminates individuals which strictly depend on host plants for stimulation of larval nutrition and of reproduction.
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  • 2
    Electronic Resource
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    Springer
    Cellular and molecular life sciences 44 (1988), S. 788-789 
    ISSN: 1420-9071
    Keywords: Yponomeuta vigintipunctatus ; Lepidoptera ; Yponomeutidae ; diapause ; photoperiodic induction curves ; low temperature influence
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Notes: Summary The long-day insectYponomeuta vigintipunctatus was subjected to various combinations of temperature and photoperiod. The photoperiodic induction curve at 10°C resembled the one at 20°C, but with a shift of the critical photoperiod towards the shorter day-length. Such unusual averting of diapause at lower temperatures in combination with intermediate long-day photoperiods has still been described in only few insect species of the temperate zone.
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  • 3
    Electronic Resource
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    Springer
    Cellular and molecular life sciences 45 (1989), S. 236-240 
    ISSN: 1420-9071
    Keywords: Lepidoptera ; semiochemicals ; sex pheromones ; host plants ; secondary plant compounds ; calling behaviour ; mate choice ; Homoesoma electellum ; Pseudaletia unipuncta
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Notes: Summary The role of host plants in the synthesis and release of lepidopteran sex pheromones is examined. Females synthesise pheromones de novo and pheromone quality is not markedly influenced by larval food sources. However, host plants may have a significant effect on different physiological and behavioural parameters associated with pheromone production. Males in some species of Nymphalidae and Arctiidae use secondary plant compounds, such as pyrrolizidine alkaloids, as a pheromone precursor. In such cases these plant compounds serve an additional role, such as protection against predation, and may reflect potential male reproductive investment. In the one instance where the effect of larval host plants on the de novo synthesis of a male sex pheromone was examined, larval nutrition did not alter either the quality or quantity of the hairpencil contents.
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  • 4
    ISSN: 1432-041X
    Keywords: Lepidoptera ; Male genital disk ; Implantation ; Regeneration ; Control of metamorphosis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary Complete and bisected male genital disks (HO) from full-grown (T9) larvae were transplanted either into larvae and pharate pupae of different age (T4, T7, T9 larvae, A1–A5 pharate pupae) or repeatedly transferred into full-grown larvae before being implanted into a final larval host. After metamorphosis of the hosts, most of the complete transplants and regenerated HO halves showed normal morphological features, but the implanted genitals from old pharate pupae (A4 and A5) were abnormally differentiated. Frequency of Regeneration. After transplanting both halves of the bisected HO into T9 hosts, three groups of results were observed: (1) each of the two halves regenerated into a complete genital organ; (2) only one half regenerated; (3) neither of the two halves regenerated. In the pharate pupae no regeneration of the implanted halves took place. If the lapse of time between the transplantation and, the onset of metamorphosis (=onset of pharate pupae phase) was long enough by transplanting into young larvae (T4) or by repeatedly transferring into old larvae and subsequent transplantation into a final larval host, all the implanted halves were able to regenerate. Size of the Implanted Genital Organs After prolonging the in vivo culture in larval hosts by implanting into young larvae or repeatedly transferring into old larvae, it was found that the regenerated genitalia grew to the same size as the complete transplants, but the size of the complete transplants increased, if at all, only insignificantly. Duration of Development of the Hosts. Regeneration of one HO half implanted into a full-grown larva caused an average delay of further development of about 2 days. An additional delay was recorded when both halves had regenerated. However, no delay was observed when HO halves implanted into young (T4) larvae regenerated, and no delay occurred in the final hosts when the repeatedly transferred halves had reached a certain stage of regeneration. The developmental capacities of the tranplanted disks and the control of metamorphosis by regenerating disks are discussed.
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  • 5
    ISSN: 1432-1432
    Keywords: Lysozyme ; Insect ; Lepidoptera ; Evolution ; Sequence
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary Sequence studies of the N-terminal halves of the lysozymes isolated fromBombyx mori, Galleria mellonella andSpodoptera littoralis (Lepidoptera) allow us to classify these enzymes among the c (chicken) type lysozymes.
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  • 6
    ISSN: 1437-5613
    Keywords: Key words Herbivory ; Plant–herbivore interaction ; Lepidoptera ; Cruciferous plants ; Vegetation texture
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract Correlation between plant size and reproductive output may be modified by herbivory in accordance with host plant density and the presence of nonhost plants. To elucidate the effects of nonhost plant density and host plant density on the intensity of herbivory and reproductive output of the host plant in relation to plant size under natural conditions, we investigated the abundance of three lepidopteran insects, Plutella maculipennis, Anthocharis scolymus, and Pieris rapae the intensity of herbivory, and fruit set of their host plant, Turritis glabra (Cruciferae). To elucidate the effects of nonhost and host plant density, we selected four categories of plots under natural conditions: low density of nonhost and high density of host plants; low density of both nonhost and host plants; high density of both nonhost and host plants; and high density of nonhost and low density of host plants. The plant size indicated by stem diameter was a good predictor of the abundance of all herbivorous species. The effects of density of nonhost and host plants on the abundance of insects varied among species and stages of insects. As the abundance of insects affected the intensity of herbivory, herbivory was more apparent on larger host plants in plots with low density of both nonhost and host plants. Consequently, the correlation between plant size and the number of fruits disappeared in low plots with density of both nonhost and host plants. In this T. glabra– herbivorous insect system, the density of nonhost plants and host plants plays an important role in modifying the relationship between plants and herbivores under natural conditions.
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  • 7
    ISSN: 1437-5613
    Keywords: Key words Community patterns ; Lepidoptera ; Route order ; Species richness ; Species distribution ; Environmental disturbance
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract Kitahara and Fujii, in 1994, analyzed the butterfly communities along a gradient of human disturbance by applying the generalist/specialist concept. Butterfly species were classified into generalist or specialist species based on their voltinism (seasonal time dimension) and potential larval resource breadth (food dimension). The community structure and species composition showed the systematic changes along the gradient. To verify the generality of those trends, we monitored five grassland butterfly communities with varying degrees of human disturbance twice a month during 1985 by the line transect method at the foot of Mt. Fuji, central Japan, and analyzed their structure in a manner similar to that employed by Kitahara and Fujii. Most results were consistent with the patterns recognized by Kitahara and Fujii. The route (community) order based on increasing human disturbance was strongly and negatively correlated with butterfly species richness but with neither butterfly species diversity (H′) nor evenness (J′). Also, the degree of human disturbance was significantly and negatively correlated with the number of specialist species, but not with that of generalists, in a community. Butterfly species richness was more strongly correlated with the number of specialist species than with that of generalists. Our analyses also showed that the generalist species were distributed more widely over the communities than were the specialists. However, in contrast to the trend revealed by Kitahara and Fujii, there was no significant difference in the population densities and in the spatial population variability between the two species groups. As a whole, our analyses confirmed the consistency of most community patterns detected by Kitahara and Fujii. The causes of the inconsistencies in some patterns were thought to be mainly the present habitat conditions with a relatively short growing season at high altitudes.
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  • 8
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    Journal of comparative physiology 182 (1998), S. 585-594 
    ISSN: 1432-1351
    Keywords: Key wordsHelicoverpa zea ; Noctuidae ; Lepidoptera ; Single-cell recordings ; Antennal neurons
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Notes: Abstract Responses of single receptor neurons in the antennae of male Helicoverpa zea to sex pheromone components and to behavioral antagonists were recorded using a cut-sensillum extracellular recording technique. Three types of sensilla were identified from sampling 325 male-specific sensilla trichodea located at the lateral edge of antennomeres. The majority of these sensilla (71%) contained a receptor neuron tuned to the principal sex pheromone component (Z)-11-hexadecenal. A second sensillar type (10%) contained a receptor neuron that responded only to (Z)-9-tetradecenal. A third sensillar type (19%) contained a large-spiking neuron tuned to the secondary pheromone component (Z)-9-hexadecenal, but this neuron also could be stimulated to equivalent spike frequencies by the same emitted amounts of (Z)-9-tetradecenal. A smaller-spiking neuron in this sensillar type responded to two compounds known to act only as behavioral antagonists, (Z)-11-hexadecen-1-ol and (Z)-11-hexadecenyl acetate, and to (Z)-9-tetradecenal. Cross-adaptation studies confirmed the presence of one large- and one small-spiking neuron in the third sensillar type. Dose-response studies correlated to collected stimuli amounts showed that the large-spiking neuron in the third sensillar type was equally tuned to (Z)-9-hexadecenal and (Z)-9-tetradecenal, whereas the smaller-spiking neuron was far more sensitive to (Z)-11-hexadecen-1-ol and to (Z)-11-hexadecenyl acetate than to (Z)-9-tetradecenal.
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  • 9
    ISSN: 1432-1351
    Keywords: Heliothis ; Noctuidae ; Lepidoptera ; Plume structure ; Behavior
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Notes: Abstract 1) Male Heliothis virescens moths flew upwind to pulsed pheromone plumes. Upon truncation of the pulsed plume males flew into clean air, turning their tracks crosswind (〉 60° relative to directly upwind direction at 0°) within an average of 0.27 s, and were casting, perpendicular to the wind-line (90°), within 0.43 s. 2) The characteristic casting flight in clean air consisted of left-right crosswind reversals, continuing for many seconds without further pheromonal stimulation. Males intercepting a single strand of pheromone during casting flight responded by surging upwind (track angles 〈 60°). The phasic surge lasted only 0.38 s before reverting to crosswind flight (〉 60°). 3) Average templates of responses in two and three dimensions were created. Males controlled their vertical deviations very tightly when in contact with pheromone but upon entering clean air, lateral and vertical excursions became much greater. 4) Males failed to sustain upwind flight to repetitively pulsed plumes generated at 〈 4 filaments/s. At the threshold frequency of 4 pulses/s we show that upwind flights were composed of reiterated surges followed by crosswind casting. As the pulse frequency increased, the tracks became straighter and the single filament cast-surge-cast template could be viewed only sporadically when, for example, a male apparently failed to intercept filaments.
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  • 10
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    Journal of comparative physiology 185 (1999), S. 131-141 
    ISSN: 1432-1351
    Keywords: Key wordsHelicoverpa zea ; Noctuidae ; Lepidoptera ; Sex pheromone ; Antagonist
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Notes: Abstract The limits of a male moth's ability to resolve closely spaced odor filaments have been investigated. Male Helicoverpa zea normally respond to their conspecific sex pheromone blend by exhibiting an upwind flight, which culminates in source contact by at least 50% of the bioassayed individuals. When loaded onto the same filter paper source containing this hitherto attractive pheromone blend, or onto a separate filter paper and co-emitted from the same pipette source with pheromone, (Z)-11-hexadecenyl acetate severely reduced upwind flight and source contact by male H. zea. A similar level of upwind flight inhibition was recorded when the antagonist (Z)-11-hexadecenyl acetate was emitted from its own point source placed 1 mm upwind of the pheromone point source, both plumes being simultaneously emitted in a continuous mode to form a confluent strand. However, (Z)-11-hexadecenyl acetate was less effective in reducing upwind flight and source contact when it was isolated and pulsed from its own source, placed 1 mm either upwind, downwind or cross-wind of a pipette source from which pheromone was simultaneously being pulsed, such that both filaments were separated in time by 0.001–0. 003 s. These results suggest that male H. zea are able to distinguish between odor sources separated by as little as 1 mm in space and 0.001 s in time.
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  • 11
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    Journal of comparative physiology 173 (1993), S. 783-799 
    ISSN: 1432-1351
    Keywords: Insect vision ; Lepidoptera ; Medulla neurons ; Optomotor stimulation ; Direction selectivity
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Notes: Abstract InManduca sexta, large tangential cells connect the medulla via the lobula valley (LoV) tract to the midbrain and the contralateral medulla. Tract neurons have been stained and recorded to determine their responses to optomotor stimulation. Neurons in the LoV-tract comprise a physiologically and anatomically heterogeneous population: 1. Motion insensitive medulla tangential (Mt) neurons arise from cell bodies in the ventral rind. Heterolateral cells arborize massively in both medullae and one or both halves of the midbrain. Mt-neurons respond to changes in light intensity. Physiological and anatomical evidence argues for their monocularity and transmission from the medulla on the side of the soma to the central brain and the contralateral medulla. 2. Motion sensitive neurons with cell bodies behind the protocerebral bridge connect the midbrain to the ipsior contralateral medulla. Direction-selective responses are characterized by excitation to motion in the preferred and inhibition in the opposite direction with maxima either in a horizontal or vertical direction. Peak values appear at contrast frequencies of appr. 3/s. The results suggest that these neurons are binocular and relay information from the midbrain to the medulla. They have been labelled as centrifugal medulla tangential (cMt) neurons. The possible roles for tract neurons in visually guided behaviour are discussed.
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  • 12
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    Journal of comparative physiology 184 (1999), S. 535-541 
    ISSN: 1432-1351
    Keywords: Key words Insects ; Lepidoptera ; Macroglossum stellatarum ; Colour vision ; Red receptor
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Notes: Abstract Hymenopterans have long been shown to choose colours by means of the spectral distribution and independently of the intensity (true colour vision). The same ability has only very recently been proven for two butterfly species. We present evidence for the existence of true colour vision in the European hummingbird hawkmoth, Macroglossum stellatarum. Moths were trained in dual-choice situations to spectral lights of a rewarding and an unrewarding wavelength. After training, unrewarded tests were performed during which the intensities of the lights were changed. The results confirm that the species has three spectral receptor types and uses true colour vision when learning the colour of a food source. If colour vision is not possible since only one receptor type is receiving input from both stimuli, the moths learn to associate some achromatic cue correlated to the receptor quantum catch, with the reward. The moths learn spectral cues rapidly and choose correctly after one to several rewarded visits even when trained to different colours in sequence.
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  • 13
    ISSN: 1432-1351
    Keywords: Threshold ; Olfaction ; Insect ; Lepidoptera ; Noctuid
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Notes: Summary 1. Responses of Trichoplusia ni HS(A) receptor neurons were measured to determine the minimum detectable concentration (absolute threshold) and the minimum detectable increment (difference threshold) for the major sex pheromone component (Z)-7-dodecen-1-ol acetate (Z7-12∶Ac). The absolute threshold was 1000-fold below the ∼10-11 M level of Z7-12∶Ac at a calling female. The Weber fraction, i.e., the ratio of the difference threshold to the stimulus concentration, declined from ∼0.8 to ∼0.06 as the concentration rose from threshold to high intensities. Relatively smaller fluctuations were detected as the stimulus increased. 2. The HS(A) responses were interpreted in relation to behavior by considering an ideal observer as approximating the central nervous system (CNS). The ideal thresholds were 3–9-fold lower than the HS(A) thresholds. 3. The ideal absolute threshold of the T. ni CNS is comparable to observed behavioral thresholds for wingflutter and taking flight. However, only a low percentage response occurs at threshold. Most males take flight at higher concentrations. Also, the ideal Weber fraction is lower than in most flight-tunnel bioassays. Yet, males respond to small fluctuations in orienting to pheromone plumes. These differences between moths and ideal observers may reflect inhibition at points in the CNS that control the flow of olfactory input.
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  • 14
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    Journal of comparative physiology 178 (1996), S. 55-61 
    ISSN: 1432-1351
    Keywords: Electrophysiology ; Lepidoptera ; Photoreceptor ; Spectral sensitivity ; Vision
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Notes: Abstract 1. The ommatidia of the butterfly Papilio have a fused and tiered rhabdom. The distal tier of the rhabdom is made up of four distal photoreceptors (R1–4), whereas the proximal tier is made up of four proximal (R5–8) and one basal photoreceptor cell (R9). 2. We first confirmed by light microscopy that the ommatidia of Papilio are not twisted, i.e. have the same spatial organization all about the longitudinal axis. The polarization method, previously applied to the distal tier, hence is applicable to identify the photoreceptor location from the peak angle of the polarization sensitivity. 3. We determined the polarization and spectral sensitivity of in total 109 proximal and basal photoreceptors in the lateral looking eye region. All of the photoreceptors were either green or red type, most of which fall into three classes as judged by the peak angles of the polarization sensitivity: around 40°, 150°, and 180° (= 0°) with respect to the dorso-ventral axis. The first two classes are formed by the proximal photoreceptors with straight microvilli oriented at the average angle of 39° (R6, 8) and 144° (R5, 7) respectively, and the third is formed by the basal photoreceptors R9 with straight microvilli oriented at 180° (= 0°). The mean polarization sensitivity (PS = maximal sensitivity/minimal sensitivity) was about 2. 4. 75% of the proximal and 48% of the basal photoreceptors were of the red type. 5. A single ommatidium of Papilio appears to contain two to four types of spectral receptors.
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  • 15
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    Journal of comparative physiology 171 (1992), S. 289-297 
    ISSN: 1432-1351
    Keywords: Electrophysiology ; Lepidoptera ; Photoreceptor ; Spectral sensitivity ; Vision
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Notes: Summary 1. A butterfly Papilio has 5 types of spectral receptors in the compound eye. The spectral sensitivity of each type peaks in the UV, violet, blue, green, and red wavelengths, respectively. The green type contains two subtypes with and without a UV secondary peak. Here we studied the localization of these spectral receptors within the ommatidium. 2. An ommatidium contains 9 photoreceptors (R1–9), each of which is one of the 5 spectral receptor types. The photoreceptors bear parallel microvilli to form a nontwisted rhabdom, and thereby the photoreceptors are polarization sensitive. 3. We first examined the microvillar orientation by electron microscopy. The microvilli of R1, 2, and 9 are oriented dorso-ventrally (0°), whereas those of R3 and 4 are parallel to the antero-posterior axis (90°). The R5–8 bear microvilli diagonally: 45° for R6 and R8, 135° for R5 and R7. 4. We then recorded spectral and polarization sensitivities from single photoreceptors. The peak angle of the polarization sensitivity (θmax) of the UV, violet, and blue receptors were around 0°, whereas that of the green receptors was around 90°. In the double-peaked green receptors, the θmax at UV was also around 90°. The red receptors showed a θmax at around 35°. The polarization sensitivity ratio (PSmax/PSmin) of the double-peaked green receptors measured at UV was around 4, whereas the ratio of other receptors was around 2. 5. We conclude that R1 and R2 are either UV, violet, or blue receptors whereas R3 and R4 are green receptors. Some R6 and R8 are red receptors. We also conclude that the UV secondary peak in the double-peaked green receptor is not simply attributable to the coupling with UV receptors.
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  • 16
    ISSN: 1432-1351
    Keywords: Carbon dioxide ; Chemoreception ; Lepidoptera ; Microclimate ; Sensory transduction
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Notes: Summary In recordings of single unit action potentials, the responses of CO2-receptors in the labial palp organ of the moth Heliothis armigera to modulation of CO2-density around a background of 350 ppm were investigated. Modulation of CO2-density by square wave changes in concentration at constant barometric pressure evokes modulation of the spike rate. Modulation of CO2-density by square wave changes in barometric pressure at constant CO2-concentration evokes responses similar to those evoked by concentration modulation. For modulation depths of less than 1.5%, the output modulation depth is linearly related to the input; at higher modulation depths the gain decreases progressively. Using sinusoidal pressure modulation, the frequency dependence of both gain and output noise was determined over a range of 0.05 to 12.8 Hz. With increasing frequency the gain progressively increases at a rate of 2.4 dB/octave up to a maximum of 63 at 3 Hz; at higher frequencies, it decreases rapidly. The threshold sensitivity of the receptors, using input noise amplitude density as a criterion, is broadly tuned, with a minimum of 1 % contrast Hz-0.5 between 0.3 and 3 Hz. Using these figures, it is concluded that the sensory organ is capable of detecting fluctuations in CO2-density of 0.14% or 0.5 ppm. The results are related to the fluctuations in CO2-density which occur in a natural environment.
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  • 17
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    Journal of comparative physiology 167 (1990), S. 309-320 
    ISSN: 1432-1351
    Keywords: Chemosensory integration ; Olfaction ; Brain ; Larva ; Caterpillar ; Manduca sexta ; Lepidoptera
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Notes: Summary 1. The physiology and morphology of olfactory interneurons in the brain of larval Manduca sexta were studied using intracellular recording and staining techniques. Antennal olfactory receptors were stimulated with volatile substances from plants and with pure odorants. Neurons responding to the stimuli were investigated further to reveal their response specificities, dose-response characteristics, and morphology. 2. We found no evidence of specific ‘labeled-lines’ among the odor-responsive interneurons, as none responded exclusively to one plant odor or pure odorant; most olfactory interneurons were broadly tuned in their response spectra. This finding is consistent with an ‘across-fiber’ pattern of odor coding. 3. Mechanosensory and olfactory information are integrated at early stages of central processing, appearing in the responses of some local interneurons restricted to the primary olfactory nucleus in the brain, the larval antennal center (LAC). 4. The responses of LAC projection neurons and higher-order protocerebral interneurons to a given odor were more consistent than the responses of LAC local interneurons. 5. The LAC appears to be functionally subdivided, as both local and projection neurons had arborizations in specific parts of the LAC, but none had dendrites throughout the LAC. 6. The mushroom bodies and the lateral protocerebrum contain neurons that respond to olfactory stimulation.
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  • 18
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    Journal of comparative physiology 168 (1991), S. 697-707 
    ISSN: 1432-1351
    Keywords: Ecdysis ; Eclosion hormone ; Manduca sexta ; Neuropeptide ; Lepidoptera ; Pupal molt ; Verson's gland
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Notes: Summary 1. Ecdysis, a behavior by which insects shed the old cuticle at the culmination of each molt, is triggered by a unique peptide hormone, eclosion hormone (EH). In pupal Manduca sexta, EH is released into the hemolymph just prior to ecdysis, and circulating hormone is sufficient to elicit this behavior. 2. Removal of the proctodeal nerves in prepupal animals eliminated the appearance of blood-borne EH, but ecdysis behavior occurred on schedule. Therefore, circulating EH is not necessary for the triggering of ecdysis. 3. In contrast, a set of dermal glands failed to show their expected bout of secretion after proctodeal nerve removal. Injection of exogenous EH rescued this secretion. Thus, circulating EH appears necessary for action on peripheral but not central targets. 4. A major reduction in EH immunostaining is seen in the proctodeal nerves just preceding ecdysis; this coincides with a 〉90% reduction in extractable EH from this structure and the appearance of circulating EH. A similar, concomitant reduction was seen in central EH cell processes, suggesting release of peptide within the CNS. 5. Antidromic stimulation of the proctodeal nerve stumps following proctodeal nerve removal triggered precocious ecdysis. This result further supports the conclusion that centrally released EH is sufficient to trigger the motor program.
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  • 19
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    Chromatographia 49 (1999), S. 699-702 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Anion-exchange chromatography ; High ph elvents ; Monosaccharides ; Carbopac PA-100
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary We have studied the elution behaviour of six common monosaccharides, fucose, galactosamine, glucosamine, galactose, glucose and mannose, on the CarboPac PA-100 column. The relative elution positions of galactose, glucose and mannose were dependent on the sodium hydroxide concentrations, a phenomenon which was likely to be the result of differential ionisation of the hydroxyl groups at ring positions two and four. The optimal resolution of the monosaccharides studied was achieved by elution with 30 mM sodium hydroxide with no appreciable loss in sensitivity at this low concentration.
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  • 20
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Meropenem in human plasma ; Solid phase extraction
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary This paper describes an HPLC method for the determination of meropenem in human plasma. The method uses solid phase extraction (SPE) of the samples and has good sensitivity, precision and accuracy. The limit of quantification in plasma samples is 0.02 μg mL−1. Calibration curves were linear over a large dynamic range, namely within 0.02–50 μg mL−1. The method was applied to the determination of meropenem levels in patients receiving meropenem, as a single dose or at steady state.
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  • 21
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Amino acids ; FMOC derivatives ; Oligopeptides
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary One classical method for quantitation of amino acids in proteins is hydrolysis of the proteins and determination of the free amino acids. Although the drastic experimental conditions necessary for complete hydrolysis always cause degradation of some of the amino acids, if mild hydrolysis conditions are used, a mixture of amino acids and oligopeptides is obtained. If these conditions are adequately tuned, the oligopeptides are almost exclusively dipeptides. For this reason we have initiated a study to find a derivatizing agent suitable for the analysis of amino acids and dipeptides by an absolute method of quantitation already tested for amino acids. FMOC-Cl was found to be a suitable derivatizing agent for this purpose.
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  • 22
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ion chromatography ; Monovalent anions determination ; Potentiometric detection ; Ion selective PVC-matrix electrode
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An all solid-state contact tubular PVC-matrix membrane electrode has been applied for potentiometric detection of inorganic and organic monovalent anions using phosphate and hydrogen phosphate eluents at low concentrations. This is a “monovalent detection method” as the selectivity of the electrode towards monovalent anions results in some other anions being undetected unless the concentration of those other anions is higher than 10−3 mol dm−3 in the sample solution injected. It takes only eight minutes to complete the separation with a good resolution. Theoretical and practical considerations are discussed, and in particular, sensitivity, linearity, detection limit and dynamic behaviour are presented. The use of an all solid-state contact bromide-selective electrode as a detector offers so far the best simultaneous sensitivity toward all anions when compared with other detection methods. Determination of Cl− and NO3 − ions in river, rain and drinking water samples without any further sample preconcentration has been successfully achieved. The detection limit is sub-ppb for most of anions in a 20 μL injection volume.
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  • 23
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; O-alkyl, O-(1-methylthioethylideneamino) phosphoramidates ; Quantitative structure-retention relationship (QSRR) ; Reversed-phase LC
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary By using factor analysis, cluster analysis and multiple linear regression methods, two parameters, FHF and ECCR, were selected from eight solute-related structure parameters as showing the best correlation with retention data. The relationship between the retention data (k) and these two structure parameters were established for ten O-alkyl, O-(1-methylthioethylideneamino) phosphoramidate compounds under the experimental conditions studied. Retention data (k) for six other compounds that have a high correlation with structure parameters were predicted using these QSRR equations. The system was evaluated by comparing the experimentalk values with the predicted ones. Good agreement was obtained between the experimental and predictedk values.
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  • 24
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    Chromatographia 49 (1999), S. 535-538 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Solid phase extraction ; Herbicides in soil ; Flupoxam
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary High-performance liquid chromatography with UV detection was used to determine the residues of flupoxam (a new herbicide) in soils. Soil samples were extracted with aqueous methanol. The soil extracts were cleaned up and concentrated using two solid phase extraction columns: a polymeric stationary phase based on a polystyrene-divinylbenzene resin (Lichrolut EN) and alumina. Recovery experiments were performed at ppb levels in spiked soil samples. The recovery was 76±1.7% for flupoxam in the range 5–100 μg kg−1 of soil. Limit of determination was 3 μg kg−1.
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  • 25
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Solid phase extraction ; Doxorubicin ; Cell culture media ; Human plasma ; Fluorescence detection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Doxorubicin is an antineoplastic antibiotic isolated fromStreptomyces peucetius var.cesius clinically used in the treatment of tumors such as lung or breast, Hodgkin's disease and various types of leukemias. The main goal of this study was to develop a simple and sensitive HPLC method with fluorescence detection for the quantitation of doxorubicin in cell culture media collected during an in vitro studies and in human plasma. Solid phase extraction (C2 silica) was applied. The experiment established five-point standard curve (1 ng mL−1 to 100 ng mL−1). The standard curves prepared in blank cell tissue media were linear over the range of doxorubicin assayed and had a mean correlation coefficient of 0.9973±9.43×10−4 and slope 0.02545±1.85×10−3. The standard curves prepared in human plasma were linear and had mean correlation coefficient of 0.997 and slope 0.01885±5.19×10−4. The limit of quantitation for doxorubicin in both specimens was arbitrarily established to be 1 ng mL−1. Intra-day variabilities were determined using 3–4 replicates of control solutions of doxorubicin (3 ng mL−1 and 30 ng mL−1) in blank plasma and cell culture media. Inter-day variabilities were determined over a four day period analyzing replicates of controls. All precision and accuracy values fell within the acceptable range.
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  • 26
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Cu(II) dimethyldithiophosphate complex ; Malathion
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    Topics: Chemistry and Pharmacology
    Notes: Summary A high-performance liquid chromatographic method has been developed for the quantitative determination of the organophosphorus pesticide malathion. The method is based on alkaline hydrolysis of malathion to dimthyldithiophosphate (DDTP) which is complexed with copper(II) and extracted in chlorofrom. The complex is injected onto a Hypersil ODS or Licrosorb sicolumn and eluted with acetonitrile:methanol:water (80∶10∶10 v:v:v) or chloroform. Detection is at 245 or 260 nm. A linear calibration curve was obtained for 24–240 μg ml−1 DDTP and a detection limit of 2.4–4.8 ng DDTP per injection. The method was applied to the analysis of malathion in commerical products after spraying on leaves. Extrction efficiency of malathion from leaves in acetone-water was also evlauted.
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  • 27
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    Chromatographia 42 (1996), S. 683-689 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chiral stationary phase ; Enantionary phase ; Enantiomer separation ; Amino acids
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Two chiral stationary phases (CSP-1 and CSP-2)) were synthesized by covalent bonding of aminopropylsilica (APS) to (a) 1-fluoro-2,4-dinitrophenyl-5-L-alanine amide (Marfey's reagent), followed by end-capping of underivatized amino groups of APS with trifluoroacetic anhydride (CSP-1), and (b) by reaction of APS with 1-fluoro-2,4-dinitrophenyl-5-L-phenylalaninetert. butyl ester, followed by cleavage of the tert. butyl ester by trifluoroacetic acid and end-capping of underivatized amino groups of APS withn-butyryl chloride (CSP-2). Both CSPs were found to be suitable for the chiral resolution of 2,4-dinitrophenyl and 3,5-dinitrobenzoyl-DL-amino acid esters by liquid chromatography using mixtures ofn-hexane andiso-propanol as eluents. Racemic 2,2,2-trifluoro-1-(9-anthryl)ethanol was also resolved on CSP-2.
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  • 28
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Column liquid chromatography ; Pesticide residues ; Surface water analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A monitoring programme based on gas chromatography (NPD, ECD) using MSD for confirmatory purposes and coupled-column liquid chromatography was applied to the analysis of pesticide residues in surface water from a predominantly agricultural area of Spain (Comunidad Valenciana). Samples analysed by means of enzyme-linked immunosorbent assay gave similar results to those obtained by GC (MSD) for the determination of total triazines. The test employed had the advantages of a simple test procedure, short analysis time and high confirmatory value. Nevertheless, the multiresidue character, accuracy and unequivocal identification of individual pesticide residues of GC (MSD) make this technique the most appropriate for environmental monitoring programmes. In this monitoring programme about 200 samples were analysed between 1993–1994. 27 different pesticides were detected in 91 of these samples. The pesticides more frequently detected were dimethoate, methidathion, endosulfan A and B, endosulfan sulphate and pirimicarb. The highest concentrations found were 39.9 μg L−1 of dimethoate, 10.6 of pirimicarb and 10.6 of methidathion.
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  • 29
    ISSN: 1612-1112
    Keywords: Capillary electrophoresis ; Column liquid chromatography ; Cefotaxime impurities ; Cross validation
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    Topics: Chemistry and Pharmacology
    Notes: Summary A micellar electrokinetic chromatography method is presented which permits separation of cefotaxime and its major related impurities. Separation was carried out at 15 kV, using 30 mM sodium dihydrogen phosphate adjusted to pH 7.2 with 5 M NaOH and which contained 165 mM sodium dodecylsulfate as electrolyte. Results obtained by capillary electrophoresis were in good agreement with those of high-performance liquid chromatography with respect to the level of the major known impurities, total impurity content and cefotaxime purity.
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  • 30
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Liquid membrane extraction ; Chlorinated phenols ; Natural water samples
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    Topics: Chemistry and Pharmacology
    Notes: Summary A sample preparation method has been developed for the determination of chlorinated phenols in water. The method is based on a supported liquid membrane extraction system connected on-line to liquid chromatography with electrochemical detection. The supported liquid membrane technique utilizes a porous PTFE membrane. The membrane is impregnated with an organic solvent which forms a barrier between two aqueous phases and enables selective extraction. The technique can easily be coupled in a flow system. In this investigation five chlorinated phenols (1–5 chlorine atoms) were extracted from natural water samples. Extraction for 30 minutes resulted in detection limits of approximately 25 ng L−1.
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  • 31
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Calcium and lead phosphate hydroxyapatite ; Globular proteins ; Colecalciferol (Vitamin D3) and related compounds ; Organophosphorus insecticides
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A qualitative study using two new stationary phases (spherical aggregates of calcium phosphate hydroxy-apatite and lead phosphate hydroxyapatite) as adsorbents in high performance liquid chromatography has achieved the separation of: a standard mixture of globular proteins; colecalciferol and related compounds (produced by irradiation and heating of provitamin D3); and a mixture of organophosphorus insecticides used in agriculture.
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  • 32
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    Chromatographia 42 (1996), S. 181-184 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ewe's milk ; Whey proteins ; Goat's milk
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary High-pressure liquid chromatography (HPLC) was used to detect added cows' milk in goat and ewe's milk. Analysis of the whey proteins enabled detection of mixtures in proportions of less than 1%. The method does not distinguish between goat and ewe's milk.
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  • 33
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    Chromatographia 42 (1996), S. 191-198 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Polymer-coated silica phase ; Polyaniline ; PAHs
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    Topics: Chemistry and Pharmacology
    Notes: Summary The use of polyaniline as a chromatographic stationary phase has been examined. In the course of this work the column packing material was prepared by coating silica particles with polyaniline chloride. The aniline monomer was polymerised directly on the surface of the silica particles using a chemical method and was characterised using elemental analysis. A series of standard test compounds were employed for chromatographic characterization. The studies revealed information on the practical utility as well as the molecular interactions that took place on the stationary phase.
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  • 34
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Gradient elution of synthetic polymers ; Polystyrene and various styrene copolymers
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Retention times in gradient liquid chromatography of synthetic polymers are often dependent on sample size. They increase with column load if the separation mechanism is governed by a solution process but decrease with increasing load if the mechanism is governed by adsorption. Since retention times independent of sample size are a prerequisite for peak identification as well as for the correct measurement of elution bands of samples with a broad distribution, measures to counteract sample-size effects deserve attention. Usually both solubility and adsorption are effective in gradient liquid chromatography of synthetic polymers. An appropriate balance of both effects is suitable for diminishing the influence of sample size on retention time of synthetic polymers. Ternary gradients allowing independent control of solubility and adsorption are promising.
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  • 35
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Supercritical fluid extraction ; Carbamate pesticides ; Soils ; Cereal
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A method for the supercritical fluid extraction of carbamate pesticides (propoxur, aminocarb, carbaryl and methiocarb) from soil and cereal samples using CO2 is proposed. Extractions were at 378 bar and 54 °C. Analytes were determined in the extracts by HPLC with fluorescence detection after post-column derivatization. Recoveries from spiked soil ranged between 39.6 and 91.7%, depending on analyte and soil components. Lowest recoveries were from sandy soils. Aminocarb could not be recovered from any soil using CO2. Recovery of aminocarb from diatomaceous earth was improved by adding methanol to the extraction cell prior to SFE, but the effect was not observed in soil samples. Recoveries for propoxur and aminocarb from spiked wheat were about 75%, and only between 30–50% for aminocarb from corn and oats, and carbaryl from wheat. Fat was coextracted using CO2 and retained in the trap together with the analytes, however, appropriate rinsing solvent allowed on-line clean-up of the extract.
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  • 36
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    Chromatographia 42 (1996), S. 199-205 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Negative ion CI mass spectrometry ; Oxidizedd-limonene ; Contact allergenic compounds
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A detailed chemical analysis and quantification of oxygen-containing monoterpenes in auto-oxidizedd-limonene was performed. Some of these, e.g. the cis- and trans-isomers of limonene-2-hydroperoxide, have previously been shown to exhibit strong contact allergenic properties. GC-MS with chemical ionization in negative ion mode was shown to be a successful method for the identification and determination of the molecular weight of chemically unstable limonene hydroperoxides. An HPLC method for isolation of individual compounds in auto-oxidizedd-limonene is presented. Two different stationary phases were used in normal phase mode, cyanopropyl- and diamino-modified silica. The method described can be used for the isolation of individual contact allergens in sensitization experiment vehicles, such as petrolatum and olive oil. This makes it possible to study whether test compounds, such as hydroperoxides, are chemically stable during a sensitization experiment.
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  • 37
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Stationary phases ; TiO2 ZrO2 AlO3 ; Separation of basic compounds
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Chromatographic properties of silica, alumina, titania and zirconia have been investigated in normal phase mode in the separation of test mixtures of basic, neutral and acidic compounds. In contrast to silica the chromatographic behaviour revealed the basic properties of the alumina, titania and zirconia surfaces. Therefore, separation of basic compounds on these packings seems very promising. Lypophilic packings have been synthesized by modification of titania, zirconia and alumina with organosilanes and polymers and tested for the separation of basic compounds and proteins. High hydrolytic stability of the modified packings was observed during separations with strong alkali and acidic eluents.
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  • 38
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    Chromatographia 39 (1994), S. 339-345 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; First-guess ; Retention optimization ; Validation
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    Topics: Chemistry and Pharmacology
    Notes: Summary A recently reported chromatographic method selection strategy has been validated using fifteen drug formulations selected randomly from the Belgium Compendium, 1992. On the basis of the hydrophobic and the acidic — basic properties of the sample components, reversed-phase was recommended as the first choice mode for all formulations. For two multicomponent formulations the range of analyte polarity dictated the need for gradient elution. The commerical software DryLab G/plus® was used for selection of optimum gradient conditions. The results obtained by both isocratic and gradient chromatography are discussed, as is the usefulness of a tailing suppressor in both modes.
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  • 39
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Size exclusion chromatography ; Pore structure ; Nitrogen sorptometry ; Zirconium oxide
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    Topics: Chemistry and Pharmacology
    Notes: Summary The pore structures of zirconium oxide particles prepared by two different methods (PICA and Oil Emulsion processes) are compared. Nitrogen sorptometry and size exclusion chromatography are used to characterize the two different types of particles. Significant and unexpected differences were found in the accessible pore volumes and the bed packing densities of the two materials. The PICA material was found to have a higher totally included and totally excluded volume than would be normally expected. The chromatographic method provides results which are more useful for the application of these materials to separation sciences.
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  • 40
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    Chromatographia 39 (1994), S. 405-408 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Electrospray mass spectrometry ; Oligonucleotides
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    Topics: Chemistry and Pharmacology
    Notes: Summary Improved HPLC and ESMS conditions have been established, allowing the separation and analysis of oligodesoxyribonucleotides by coupled HPLC-ESMS.
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  • 41
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ion-exchange chromatography ; Protein purification ; Pentosan polysulfate displacers ; Dextran sulfate displacers
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Experimental studies were carried out to investigate the utility of pentosan polysulfate as a low molecular weight polyelectrolyte displacer for the purification of proteins in anion-exchange displacement systems. In addition, the influence of mobile phase salt concentration on displacer efficacy, protein-protein resolution, and displacement development were studied for several anionic displacers. It was found that while large polyelectrolytes (50 kd dextran sulfate) were efficient displacers for a wide range of salt concentrations, relatively small polyelectrolytes (3 kd pentosan polysulfate) were seen to act as an efficient displacer only under conditions of high salt micro-environments. In addition, for proteins exhibiting similar affinities, zone mixing at the protein-protein boundary was found to be quite sensitive to the salt concentration. Finally, displacement chromatography was successfully implemented for the separation of proteins from milk whey.
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  • 42
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    Chromatographia 39 (1994), S. 427-430 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Microcystins RR and LR ; Solid phase extraction ; Cyano cartridges
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    Topics: Chemistry and Pharmacology
    Notes: Summary A new method for the determination of microcystins PR and LR in cyanobacterium was developed using cyano-type prepacked cartridges. The microcystins were extracted with 10% acetic acid and the extract applied to a Baker 10 cyano cartridge. After elution from the cartridge with 0.5M acetic acid-acetonitrile (1∶9) the microcystins were determined by HPLC. Better recoveries and chromatograms were observed than with ODS cartridges.
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  • 43
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    Chromatographia 42 (1996), S. 318-322 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Adenosine in blood ; Isocratic elution ; Stop-solution
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Due to manifold physiological and cardioprotective actions of adenosine, the demand for a simple but accurate method to determine its concentration in plasma is increasing. The aim of this study was firstly to develop a simple isocratic method instead of the gradient elution or peak-shifting techniques used earlier and secondly to check conflicting data on the composition of “stop-solution”, added to the sample in order to prevent changes in adenosine concentration. Isocratic elution improved signal to noise ratio and concentrations of 100 μmol L−1 dipyridamole and 2.5 μmol L−1 erythro-9(2-hydroxy-3-nonyl)adenine in the blood sample effectively prevented both adenosine formation and degradation, even without the use of a 5′-ecto-nucleotidase inhibitor. Lowering the concentration of dipyridamole to 25 μmol L−1 caused more than a tenfold increase of adenosine concentration in two out of five cases and even 100 μmol L−1 dipyridamole alone is not sufficient to inhibit adenosine deaminase in blood samples.
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  • 44
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    Chromatographia 42 (1996), S. 401-404 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Hummel Dreyer method ; Sulfinpyrazone ; Bovine serum albumin ; Scatchard-Rosenthal plot
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    Topics: Chemistry and Pharmacology
    Notes: Summary Hummel-Dreyer method was used to study the binding of sulfinpyrazone to bovine serum albumin. The technique involves our newly developed internal calibration method with the elution pattern consisting of two positive peaks and with the integrator to evaluate the area of second peak. From the area of the second peak the numerical value ofL b (the amount of drug bound to protein) was calculated. Sctachard-Rosenthal plot was used to estimate the binding parametersn i (the number of binding sites) andk i (the binding constants). The results are compared with those obtained by equilibrium dialysis.
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  • 45
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Precolumn derivatization ; Dansylhydrazine ; Fluorescence detection ; Tacrolimus (FK 506) in blood
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A sensitive and selective liquid chromatographic method, using precolumn derivatization with dansylhydrazine followed by fluorescence detection, has been developed for the determination of tacrolimus (FK 506) in whole blood. After haemolysis, whole blood samples are extracted with diethyl ether and derivatized. After on-line removal of excess dansylhydrazine on a C18 precolumn, the derivative is loaded on to a C18 clean-up column, and a heart cut is subsequently transferred to a graphitized carbon column, where the final separation takes place. The method requires 1 ml of sample and has a limit of quantitation of 3 ng/ml. At the 15 ng/ml level the precision isca 10%, and the response is linear from the limit of quantitation toca 200 ng/ml of FK 506 in whole blood. The capacity of the method is 50 samples/day and about 1000 1-ml samples can be analyzed without changing either clean-up or separation column. Finally, the applicability of the method for therapeutic drug monitoring is shown.
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  • 46
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; New bonded phases ; 13C and29Si CP-MAS NMR ; DRIFT ; ESCA
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    Topics: Chemistry and Pharmacology
    Notes: Summary A variety of olefins were bonded to silaceous supports through a hydride modified substrate. The products were then examined by13C and29Si solid state-NMR with cross-polarization (CP) and magic angle spinning (MAS). Information about the surface was also obtained by diffuse reflectance infrared Fourier transform spectroscopy (DRIFT) and the related photoelectron spectroscopic technique (ESCA). Carbon analysis on bonded silicas was carried out and surface coverage was calculated. Confirmation of the organic groups bound to the silica support was possible. The hydride intermediate is shown to be a versatile material for bonding a wide variety of organic moieties to silica surfaces.
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  • 47
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Glucocorticoids ; Betamethasone and dexamethasone ; Pharmaceuticals ; Tablet preparations
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An HPLC method for the simultaneous determination of the glucocorticoids betamethasone and dexamethasone is described. The method based on the separation of these compounds using a binary watertetrahydrofuran mobile phase and a reversed-phase Hypersil C18 column, was applied to the determination of betamethasone and dexamethasone in tablets.
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  • 48
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    Chromatographia 39 (1994), S. 557-563 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Copoly(styrene/methyl methacrylate) ; Gradient elution ; Precipitation chromatography of polymers ; Solubility of polymers
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Copolymers from styrene and methyl methacrylate (MMA) were separated by both normal and reversedphase gradient chromatography. Both modes could be performed by sudden-transition gradients where the polymers were injected into a non-solvent whose polarity was either rather low (e.g.,n-heptane) or high (e.g., acetonitrile). Then the solvent strength of the starting eluent was rapidly increased to a given level by addition of dichloromethane. Under properly defined conditions, the sample components still remained on the column. Elution could be triggered off by the steady addition of another non-solvent whose polarity was opposite of that of the starting non-solvent. Thus, the mixture of five copolymers with MMA content ranging from 14 to 84% could be separated on a polar cyanopropyl column by injection inton-heptane and elution through acetonitrile (normal phase mode) and on a RP C18 column by injection into acetonitrile and elution throughn-heptane (reversed-phase mode), provided that in both modes about 30% dichloromethane was added to the starting non-solvent. The elution sequence in the reversed-phase mode was opposite to that in the normal-phase mode, obeying the approved polarity rules of chromatography in both cases.
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  • 49
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Tryptophan ; Chiral separations ; Diode-laser polarimetric detection
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    Topics: Chemistry and Pharmacology
    Notes: Summary The combined utilization of photometric, fluorimetric and polarimetric detection liquid chromatography detectors in series for the identification and quantification of D-tryptophan and L-tryptophan was evaluated. Detection limits of about 1 μg were established with the range of linearity extending to about 100 μg. The relative standard deviation of the D-form and L-form tryptophan were 7.32 and 4.22%, respectively. The amount unknown of tryptophan enantiomers in the different mixtures was determined with an accuracy of 1.58% at the 40 μg injection level.
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  • 50
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    Chromatographia 42 (1996), S. 499-505 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Hop bitter acids ; Supercritical fluid extraction ; On-line-1H NMR coupling
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A supercritical carbon dioxide hop extract has been analysed using on-line coupling of high performance liquid chromatography (HPLC) with1H nuclear magnetic resonance (NMR) spectroscopy. For the first time high quality NMR spectra of the six major hop bitter acids were recorded by employing the stopped-flow detection mode. The resolution of the spectra obtained is similar to that of conventionally recorded spectra. All data are in agreement with the known structures.
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  • 51
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Thiol drugs ; Pre-chromatographic derivatization ; 1,1′-[ethenylidenebis(sulfonyl)]bis-benzene reagent
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The use of 1,1′-[ethenylidenebis(sulfonyl)]bis-benzene as a pre-chromatographic reagent for LC analysis of thiol drugs is proposed. The reagent reacts rapidly (2 min) under mild conditions (pH 7.5, ambient) with thiol drugs and the resulting adducts can be chromatographed under reversed-phase conditions (C-18 column). Excess reagent can be removed from the reaction mixture by simple liquid-liquid extraction with chloroform. The HPLC method using UV detection was successfully applied to the analysis of reduced glutathione (GSH), N-acetylcysteine, N-2-mercaptopropionylglycine and captopril in their commercial formulations.
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  • 52
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Micellar electrokinetic capillary electrophoresis ; Tetrahydrocarbazole derivatives ; β-Cyclodextrin ; Taurodeoxycholate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary 2,3,4,6-tetra-O-acetyl-β-D-glucopranosyl isothiocyanate derivatives of a number of basic compounds, containing one chiral center, have been prepared. The indirect resolution of enantiomers was achieved with a high separation efficiency by capillary electrophoresis, using a sodium taurodeoxycholate/β-cyclodextrin system. This methodology was found to be superior to the resolution of the same derivatives by reversed phase HPLC analysis. A possible mechanism for stereoselectivity is described.
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  • 53
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Un-sulphated and sulphated surfactants ; Oligoethyleneglycol nonylphenyl ethers
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Retention behaviour of un-sulphated and sulphated, oligoethyleneglycol nonylphenyl ether, anionic surfactants was investigated in normal-phase LC systems with chemically bonded amino stationary phase in organic mobile phases containing water and cetyl trimethylammonium bromide (CTAB). Addition of water to the mobile phase improves efficiency of separation and linearity of the dependences of logk′ versus number of oxyethylene units in the sulphated oligomers, so that it is possible to describe simultaneous effects of this number and of the concentration of CTAB on retention by a simple equation. In this system, it is possible to separate lower sulphated and un-sulphated oligomers in a single run in 10–15 min under isocratic conditions.
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  • 54
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Electrothermal atomic absorption spectrometry ; Vitamin B12 analogues ; Cobalamins and cobalt ; Meat
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The coupling of liquid chromatography and electrothermal atomic absorption spectrometry (LC-ETAAS) lowers the detection limit for identification of vitamin B12 analogues. Cobalamins and aqueous cobalt (II) were separated by reversed-phase liquid chromatography using a linear gradient: 26∶74 (v/v) methanol:0.05 M phosphate buffer (pH 4.2) to 50∶50 mixture over 8 min. The vitamins were quantitatively determined in the column effluent by measuring total cobalt by ETAAS. The analysis of meat and liver extracts by LC-ETAAS showed that the matrix did not interfere with the determination of cobalt. Hence, recoveries of cobalt in spiked meat and liver samples were satisfactory.
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  • 55
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Anion-exchange chromatography ; Benzhydrylamine resin ; pK a
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary For better evaluation of the potential of benzhydrylamine resin (BHAR), used as a solid support for peptide synthesis, as a novel anion-exchange resin, the pK a of its amine group was estimated by microscopic measurement of the sizes of the dry and swollen beads. Using the volume of the bead occupied by the solvent (as a percentage) as the swelling parameter, a plot of the degree of swelling of BHAR loaded with 2.4 mmol g−1 amine groups against the pH of the medium produced a decreasing sigmoidal-type curve with increasing pH. By considering the point of inflection of the curve, a pK a value of approximately 7.5 was estimated for the amine group of the BHAR. The same approach was also applied to the lysyl derivative of the BHAR (Lys-BHAR) and pK a values around 6.5 and 10.0 were obtained for the α and ε amine groups, respectively.
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  • 56
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Sterols, tocopherols, retinols and carotenes ; Dairy products
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary We have previously described a normal-phase HPLC method for the simultaneous determination of α, β, γ and δ tocopherol, thecis andtrans isomers of retinol, and total carotenes in different Italian cheeses and milk. In this paper we describe a reversed-phase HPLC method using solely methanol as the mobile phase for the determination of α-tocopherol, β-+γ-tocopherols, total retinols, cholesterol, β-sitosterol, campesterol and stigmasterol, and α- and β-carotene. The method developed has been applied to some new dairy products such as natural Quark, with olive, basil or banana and to processed cheese with tomato and the results have been compared with the corresponding results obtained by the normal-phase method. The conclusion is that more complete evaluation of the tocopherol, retinol, carotene and sterol content of dairy products, especially when vegetables and fruits are present, is necessary and can be obtained using both the normal- and reversed-phase HPLC methodologies.
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  • 57
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Micellar vs. reversed phase separation ; Thiram in river water ; Dithiocarbamate fungicides
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary After a comparative study of conventional reversed phase and micellar liquid chromatography a method is described for the determination of the fungicide thiram in river water based on the use of micelles of CTAB. The method involves the extraction/concentration of thiram with a C18 cartridge followed by separation on a C18 reversed-phase column with a mobile phase of 20% (v/v) acetonitrile/0.01 M CTAB in phosphate buffer (pH-6.3), and detection at 254 nm. The method allows the determination of thiram in the presence of other water-soluble dithiocarbamate fungicides (nabam, ziram and ferbam) with a limit of detection of 36 pg mL−1 for a typical 20-fold preconcentration.
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  • 58
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Diode-array detection ; Particle beam mass spectrometric detection ; Pesticides in water ; On-line solid-phase extraction (SPE)
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A group of pesticides has been determined by liquid chromatography with diode-array detection (DAD). The coupling of a particle-beam (PB) mass spectrometer to the outlet of the DAD enabled the identities of the pesticides to be confirmed from mass spectra obtained by electron impact ionization. On-line trace enrichment of 200 mL of sample with a PLRP-S precolumn enabled most pesticides to be determined in real samples at levels between 0.2 and 5 μg L−1 and with limits of detection (LOD) between 0.05 and 0.5 μg L−1. In the analysis of real samples, one of the pesticides studied was determined by DAD and its identity was confirmed by comparison of PB mass spectra. The use of PB-MS also enabled the detection of non-target compounds.
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  • 59
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Hexamethyldisiloxane ; Mobile phase component ; Silica column
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Hexamethyldisiloxane (HMDX) has been evaluated as a modifier solvent for the normal phase separation of substituted naphthalene componds as well as aromatics such as nitrobenzene, acetophenone, benzonitrile, and aniline. It is found to be a weaker eluting solvent than n-butyl ether and other commonly used normal phase solvents filling a niche in the eluotropic series. HMDX exhibited an unusual retention factor (k′) profile as a function of mobile phase composition in hexane. In a range from 0 to 40 %, thek′ values remained quite constant with increasing HMDX composition. As the concentration of HMDX progressed to 100 %, thek′ values actually increased in a generally linear fashion. This trend ink′ is due to longer solute retention not just a change in the retention time of the unretained component. Although slight silanization of the silica column may occur with initial use of HMDX, retention of these analytes on a commerical C-1 silica column is much lower with no positivek′ slope with increasing HMDX. The chromatographic data provide evidence that HMDX is likely adsorbed to the silica surface and a solute partitioning mechanism may be operative.
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  • 60
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    Chromatographia 43 (1996), S. 654-658 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Thin-layer chromatography ; Ion-pairing ; Sulfonamides ; NH2-Modified stationary phase
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Thin-layer and column high-performance liquid chromatography based on amino propyl-modified silica gel using aqueous and non-aqueous mobile phases containing organic modifier and cationic or anionic ion-pairing reagents were used for the determination ofR F andk values of some sulfonamides. The influence of the different organic modifiers and ion-pairing reagents on retention has been compared.
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  • 61
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Polycyclic aromatic hydrocarbons ; Waste waters ; Sewage sludge
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A modified solid-phase extraction technique using sonication of the adsorbent material instead of the elution normally applied has been compared with two conventional liquid-liquid extraction procedures for the determination of the 16 EPA PAHs in municipal waste waters by means of HPLC coupled with fluorescence detection. Liquid-liquid extraction with cyclohexane proved to be the most efficient and simplest procedure. Clean-up of the waste-water extracts was not considered necessary, because of the high chromatographic resolution of the column and the selectivity of the fluorescence detector. Different organic solvents were also compared for ultrasonic extraction of PAHs from sewage sludge. The best results were obtained by use of acetonitrile. Clean-up of sewage-sludge extracts was not found necessary for accurate quantification of the major PAH components with fluorescence detection. The precision of the whole analytical procedure from extraction to the final determination of PAHs was satisfactory for both waste-water and sewage-sludge samples.
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  • 62
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    Chromatographia 43 (1996), S. 117-123 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ion-exchange chromatography ; Ion-exchange mechanism ; Optimization of alkali and alkaline earth separation ; Crown ether complexing reagents
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The elution behavior of alkali and earth alkaline cations has been studied on a newly synthesized weak cationexchanger (WCX). Applying this stationary phase isocratic separation of these cations is possible. The dependence of retention on competing ion concentration is described via a simple model. The influence of crown ethers as well as organic eluent additives on selectivity and peak efficiency is demonstrated. With optimized separation such cations can be determined with detection limits of about 0.5 ppm using a conductivity detector without ion suppression.
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  • 63
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Tandem mass spectrometry ; Fumonisin in corn products ; Electrospray-ionization (ESI) ; Selected rection monitoring (SRM)
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A new method has been developed for qualitative and quantitative analysis of fumonisin FB1 and FB2 in corn and corn products. After extractive sample preparation followed by solid phase extraction using a strong anionexchanger, highest selectivity and sensitivity was achieved by high-performance liquid chromatography-electrospray-ionization, tandem mass spectrometry (HPLC-ESI-MS-MS) analysis combined with selected reaction monitoring (SRM). With deuterated fumonisin FB1-d6 as internal standard the routine quantitation limit for FB1 was set at 400 pg (0.8 ng g−1 sample) with a signal-to-noise ratio of 10∶1. Almost all corn grit and corn meal samples under study were found to be contaminated with fumonisin FB1 and FB2 in concentrations ranging from 1 to 200 ng g−1. Lower fumonisin levels were found in cornflakes, popcorn and baby food, while no fumonisins were detected in canned sweet corn.
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  • 64
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; On-line liquid chromatography-mass spectrometry ; Neutral and acidic cannabinoids ; Hashish samples
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary This paper reports the use of liquid chromatography for the separation and determination of the major cannabinoids extracted from hashish samples. The direct coupling to the mass spectrometer enables the selective identification both of neutral and acidic cannabinoids. The developed method does not require any preliminary derivatization and should, therefore, be of interest in forensic analysis for simple and unequivocal determination of hashish constituents.
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  • 65
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ruthenium diimine complexes ; Inorganic synthesis ; Kinetics monitoring
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The synthesis of the complex [(bpy)2Ru(Im)2]2+ (bpy=2,2′-bipyridine; Im=imidazole) has been monitored by reversed-phase HPLC. The analytical results obtained during the reaction have shown that it is feasible to identify and isolate the [(bpy)2RuIm(H2O)]2+ complex as a reaction intermediate. The optimization of the synthetic procedures for these two species has been established and the compounds have been obtained in high purity. The use of HPLC has enabled complete analytical control of the synthesis of the [(bpy)2RuL2]2+ class of compounds, enabling the identification of reaction intermediates.
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  • 66
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Desacetyl diltiazem hydrochloride stereoisomers ; Chiralcel OF ; Chiral inversion ; Epimerization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Direct resolution of four stereoisomers of the related compound of diltiazem hydrochloride, namely desacetyl diltiazem hydrochloride, was studied by both normal and reversed-phase chiral HPLC. The four stereoisomers were completely resolved on a Chiralcel OF column. The technique developed was applied to a chiral inversion study of desacetyl diltiazem hydrochloride. This inversion was observed neither in the solid state, in aqueous solution at 100°C for 3 h nor under visible light for 10h, but was observed in aqueous solution under UV irradiation. The (+)-(2S, 3S)-cis-desacetyl diltiazem hydrochloride degraded with a half-life of 1.9 h in aqueous solution under UV and epimerized to (+)-(2R, 3S)-trans-desacetyl diltiazem hydrochloride. Similarly, (+)-(2S, 3S)-cis-desacetyl diltiazem hydrochloride degraded about three times faster than diltiazem hydrochloride. Reverse epimerization of (+)-(2R, 3S)-trans-desacetyl diltiazem hydrochloride to (+)-(2S, 3S)-cis-desacetyl diltiazem hydrochloride was not observed. The overall degradation was the result of two competitive processes, the epimerization and the decomposition of the benzothiazepin ring. The degradation and epimerization rate of (+)-(2S, 3S)-cis-desacetyl diltiazem hydrochloride in solution under UV depended upon the solvent, the aqueous pH, and concentration.
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  • 67
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chemically bonded silica gel ; Mixed solvents ; Steroids
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The chromatographic behaviour of 30 estradiol and estrone derivatives has been studied on diol, amino- and cyanopropyl silica gel stationary phases with non-aqueous mobile phases. The slopes of linear relationships between the logarithm of the retention factor and logarithm of the volume fractions of the polar components of the binary eluents have been calculated and are discussed in relation to the characteristics of the solute, eluent and stationary phase. An equation for testing the separation efficiency of stationary phases has been derived.
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  • 68
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Experimental design ; Direct chiral resolution ; Omeprazole ; Hydroxy-omeprazole
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A strategy for the optimisation of direct chiral separation of omeprazole and a metabolite, hydroxi-omeprazole, in reversed phase liquid chromatography is described. A factorial design was used, where mobile phase pH, concentration of a mobile phase modifier, ionic strength and column temperature were tested as the variables and enantioselective retention, column efficiency and asymmetry factor as the responses. The experimental results were evaluated with multivariate analyses, which demonstrated that the column temperature and content of mobile phase acetonitrile were by far the most important variables. The enantiomers of omeprazole and one of its metabolites were baseline resolved within 15 minutes. The optimised chromatographic system was used for a separation of the enantiomers of omeprazole and its main metabolite in a patient plasma sample.
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  • 69
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    Chromatographia 44 (1997), S. 19-24 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Cisplatin stability ; Cisplatin metabolites ; Platinum phosphato-derivatives
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Althoughcis-dichlorodiammineplatinum(II) (cisplatin or CDDP) is widely used for the treatment of several kinds of tumour, its stability and metabolism in biological fluids have not been completely elucidated. Conditions in which mobile phases of formic or phosphoric acids interact with platinum derivatives during chromatographic separation performed by high performance liquid chromatography on-line with inductively coupled plasma-mass spectrometry (ICPMS) are investigated. During chromatographic separation of CDDP the formic acid mobile phase does not interact with CDDP itself nor with its hydrolysis products. In contrast, the phosphoric acid mobile phase interacts, not with the CDDP itself, but with its hydrolysis products which are present only in an aged aqueous solution, to generate two platinum phosphato-derivatives. This study suggests that the phosphoric acid has greater affinity for the CDDP hydrated complexes than formic acid and the latter is more appropriate for the study of cisplatin behavior in aqueous and biological media.
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  • 70
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chemiluminescence detection ; Tiopronin ; Thiols
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary In previous pharmacokinetic studies tiopronin, a drug used for effective treatment of cystinuria and rheumatoid arthritis, and its metabolite 2-mercaptopropionic acid were analysed by conventional liquid chromatography with pre- and post-column derivatization and UV detection. Now a novel HPLC-coupled chemiluminescence-flow-injection analysis (CL-FIA) method has been developed for the determination of tiopronin and 2-mercaptopropionic acid in urine. The method is based on chemiluminescence from a Ce(IV) oxidation system sensitized by quinine, as proposed earlier by this group, and flow-injection analysis. The method, which has the advantages of high sensitivity and selectivity, simple sample treatment and prompt production of results, has also been preliminarily adapted for pharmacokinetic study of tiopronin in urine.
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  • 71
    ISSN: 1612-1112
    Keywords: Thin layer chromatography ; Column liquid chromatography ; Radioimmunoassay ; Cortisol ; Guinea pig ; Urine
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary In order to collect urinary samples from unrestrained guinea pigs, animals were kept in their familiar home cages with wood shavings for bedding. Cortisol was removed from shavings by a simple washing step, and an attempt was made to measure its concentrations by high performance thin-layer chromatography (HPTLC), high performance liquid chromatography (HPLC), or thin layer chromatography/radioimmunoassay (TLC-RIA). After intramuscular administration of 25 mg cortisol, cortisol excretion increased from about 20–30 μg/day to 400–500 μg/day (HPTLC: 531 μg/day, HPLC: 493 μg/day; TLC-RIA: 394 μg/day). Similarly, the treatment of the animals with 20 IU ACTH resulted in an augmented cortisol excretion, with mean values of 294 μg/day (HPTLC), 256 μg/day (HPLC) and 143 μg/day (TLC-RIA), respectively. The present study shows, for the first time, that cortisol excretion in unrestrained laboratory animals can be determined. Whilst the cortisol values measured by HPTLC and HPLC agree, the amounts measured by TLC-RIA were significantly lower. These differences are probably due to the presence of substances in urine or shavings which interfere with the radioimmunological determination. Hence, cortisol should be determined either by HPTLC or HPLC. Beside having a desirable specificity, these methods are more suited than TLC/RIA for steroid analysis since they confer the possibility of measuring additional steroids (e.g. precursors and/or metabolites of cortisol) in a single urine extract. This is especially the case for the HPTLC method since substances can be transformed into fluorescent derivatives.
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  • 72
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Column-switching systems ; Restricted-access media precolumns ; Mobile phase composition
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Various mobile phases including phosphate buffer, pure water and five kinds of biological buffers (pH around 7) were systematically studied in terms of their ability to clean-up plasma matrix on precolumns of restrictedaccess media in a column-switching system. The necessary washing time, buffer pH, type and content of organic modifier were evaluated with respect to plasma elution profiles on restricted-access media precolumns. The influence of different mobile phases on the recovery of plasma matrix from alkyl-diol silica precolumns was studied by means of a scanning spectrophotometer. Our results show that phosphate buffer near physiological pH with small amounts of 2-propanol or acetonitrile was prefereble for direct injection of large plasma volumes (500 μL). More than 93% of the proteins in a plasma matrix can be recovered within 3 min from the alkyl-diol silica C18 column (25 mx 4 mm I.D.) as measured at 280 nm for all selected mobile phases except for tris (hydroxymethyl) aminomethane buffer, from which only about 88% was obtained.
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  • 73
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    Chromatographia 44 (1997), S. 619-622 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Boldine in pharmaceuticals
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A method is proposed for extraction, separation, identification and quantitative measurement of boldine (I) in pharmaceuticals. The extraction of (I) from the matrix (syrups, tablets, extracts) was realized with aqueous ammonium chloride (0.02 M, pH=3.0 with perchloric acid) and the clean-up of the extract was performed by solid-phase extraction by means of cartridges containing a strong cation-exchange sorbent, from which (I) was eluted with aqueous ammonium chloride (1 M, pH=10.0 with ammonia). The final eluate was examined by HPLC. Chromatography was performed on a C-8 column with a gradient elution from 15:85 to 30:70 of acetonitrile-water containing 0.1 M sodium perchlorate (pH=3.0), in 20 min. A diode array detector was used at 302 nm for detection. The method gives recovery values greater than 98% and the reproducibility is within 6.0%.
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  • 74
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    Chromatographia 40 (1995), S. 9-14 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Porous graphite ; Chiral stationary phase ; Copper complexation chromatography ; Amino acids ; Hydroxy acids ; Adsorbed stationary phases
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A new type of chiral stationary phase has been prepared by coating porous graphite with a near-monolayer of an adsorbed enantiomeric modifier which then acts as an adsorbed stationary phase. The most effective modifiers are L- or D-isomers of N-(2-naphthalene-sulphonyl)-phenylalanine (NS-Phe). Conveniently 80% of monolayer coverages, corresponding to 1.2 μmol m−2, are achieved by adsorption of NS-Phe from methanolic solution. Enantiomeric separations by complexation with cupric ion show base-line resolution of α-amino and α-hydroxy acids with separation factors up to 2. Identical separations are achieved with chiral phases made from the L- and D-isomers of NS-Phe except that the elution orders of enantiomers are inverted. Reduced plate heights are around 5 and the adsorbed chiral phases are extremely stable, retention ratios being unchanged after passage of 7000 column volumes of eluent. A mechanism of retention is proposed, which fits the experimental observations.
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  • 75
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Environmental samples ; Azines and diazines
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Several heterocyclic compounds have been investigated by HPLC on RP-8 and RP-18 with methanol-water mixtures as mobile phase. The chromatographic systems developed showed good selectivity for determination of azines and diazines. Pyridine and quinoline have been determined in environmental samples and in food. Samples for analysis were preconcentrated by solid phase extraction on-column with octadecyl silane packing.
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  • 76
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Enantioseparation ; ChiralcelR OJ ; Anti-HIV agents ; Thiazolo-benzimidazoles
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A series of enantiomeric 1H,3H-thiazolo[3,4-a] benzimidazoles with anti-HIV activity has been stereospecifically analyzed. The enantiomeric resolution has been carried out by means of an HPLC method using a column of cellulose tris-(4-methyl-phenylbenzoate) ester adsorbed on macroporous silica gel (ChiralcelR OJ).
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  • 77
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    Chromatographia 40 (1995), S. 51-57 
    ISSN: 1612-1112
    Keywords: Column electrophoresis ; Column liquid chromatography ; Phenolic lignin degradation compounds ; Sugar degradation products ; Quantitative analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A method for the quantitative analysis of phenolic lignin degradation products by capillary electrophoresis (CE) with on-column UV detection has been developed. The liquid biomass solutions contain low molecular hemicellulosic sugars and phenolic lignin degradation products with various degrees of polymerization. Special attention has been paid to the monomeric phenolic components of lignin degradation fragments, e.g. derivatives of phenolic acids, aldehydes, and alcohols. Uncoated fused silica capillaries and borate-phosphate buffer systems at moderate pH conditions were used in order to separate the compounds of interest. To provide validation of the method, the same samples were analyzed independently by HPLC using gradient elution on a RP-C18 column. As sugar degradation fragment, furan-2-carboxylic acid was detected.
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  • 78
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    Chromatographia 40 (1995), S. 85-90 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Phenolic compounds ; Ion-pair solid phase extraction ; On-line trace enrichment
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Two packing materials, C18 and PLRP-S, are studied for on-line trace enrichment of phenolic compounds in water. Various precolumns of different internal diameter are also tested and the addition of an ion-pair reagent to increase retention and thus, breakthrough volumes of phenolic compounds, is studied. Best results are obtained when a PLRP-S precolumn is coupled on-line with a C18 analytical column and DAD detector. Addition of TBA considerably increases breakthrough volumes. In contrast, when a C18 precolumn is used, breakthrough volumes are lower and it is impossible to determine TCP and PCP, under the experimental conditions used, because of interference of other nonpolar compounds in the samples. The performance of the system is evaluated with river and tap water and the preconcentration of 10 ml of sample in a PLRP-S precolumn involves a linear range between 1 μg 1−1 and 20 μl−1 and limits of determination between 0.5 μg l−1 and 1 μg l−1 are obtained.
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  • 79
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    Chromatographia 40 (1995), S. 99-101 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; High temperature open-tubular columns ; Solvent make-up ; Acetophenone oxidation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Acetophnone, a substance stable at room temperature, is readily oxidizes in a high temperature open tubular liquid chromatographic system by the residual oxygen in the mobile phase. The oxidation product is less UV absorptive and detection sensitivity decreases greatly. To prevent the oxidation, through degassing of the mobile phase is necessary.
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  • 80
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chiral resolution of amino acids ; Pre-column derivatization ; Fluorescent chiral tagging reagents ; Stereochemical purity
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Derivatization of amino acid enantiomers with fluorescent chiral Edman-type reagents, 4-(3-isothiocyanatopyrrolidin-1-yl)-7-nitro-2,1,3-benzoxadiazole [R(−)- and S(+)-NBD-PyNCS] and 4-(3-isothiocyanatopyrrolidin-1-yl)-7-(N,N-dimethylaminosulfonyl)-2,1,3-benzoxadiazole [R(−)-and S(+)-DBD-PyNCS], yields corresponding diastereomers separable by reversed-phase HPLC on normal achiral columns. The resolved diastereomers were detected fluorometrically at 530 nm with excitation at 490 nm for the NBD-PyNCS derivatives and at 560 nm with excitation at 450 nm for those derived from DBD-PyNCS reagents. This HPLC-derivatization method was used for evaluation of stereochemical purity for some synthetic commercial peptides. The enantioanalysis was reliable down to 0.05% racemization of the amino acid residues and a quantity of 100 μg peptide sample was usually enough for the analysis. Two acid hydrolysis methods, i.e. the standard procedure with constant-boiling hydrochloric acid (HCl) and a rapid vapor-phase procedure with HCl-trifluoroacetic acid (TFA) mixture, were compared. The later was found to be unsuitable owing to increased racemization of the amino acid residues during the hydrolysis. Judging from the results obtained for proline and leucine residues, most of the tested peptides including biologically active peptides, such as neurotensin, [d-Ala2,d-Leu5]-enkepharin and morphine tolerance peptide, possessed stereochemical purities higher than 98%. Influence of structural features of the peptides on the racemization of the amino acid residues was found to be significant.
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  • 81
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Preservatives-antioxidants ; Eluent pH ; Retention and separation factors
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary In this paper the dependence of eluent pH on the efficiency of separation in RP-HPLC is described. Preservatives-antioxidants, esters ofp-hydroxybenzoic acid (methyl, ethyl, propyl and butyl parabens), sorbic acid, butylated hydroxyanisole (BHA), butylated hydroxytoluene (BHT), propyl gallate (PG) and L-ascorbic acid (Vitamine C) were investigated by reversed-phase high-performance liquid chromatography, utilising isocratic elution with UV detection. The mobile phase composition (methanol-water v/v containing 1% acetic acid), was varied in order to obtain the best separation. For all substances analysed the pH, pKa and the fitted pKa values were calculated in different mixtures of mobile phases using the graphical method of Charlot and Trémillon [1]. The retention factors (k) and the separation factors (α) were also calculated.
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  • 82
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Transchelation ; Zinc pyrithione and related compounds ; Antidandruff formulations
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An analytical procedure has been developed for the determination of zinc pyrithione in antidandruff formulations. Zinc pyrithione was converted into a stable copper complex and then analysed by reversed-phase HPLC. The proposed method allows the separation of the analyte from related pyrithiones and therefore is able to verify the compliance of cosmetic preparations with current legislation.
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  • 83
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Mass spectrometric detection ; Fast atom bombardment ionization ; Serum bile acid ; Rat bile
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary In order to analyse bile acids in biological matrices, e.g. rat bile and human serum, high performance liquid chromatography (HPLC) was coupled to continuous-flow fast atom bombardment mass spectrometry (CFFAB-MS). A gradient elution system which had already proved to be well suited for the quantitative determination of conjugated bile acids in bile was modified to allow HPLC-CFFAB-MS-coupling. Due to the sensitivity of this coupling method it is possible to obtain more information about the biliary bile acid pattern and species-specific secondary bile acids. Furthermore, we were able to identify obviously unknown bile acid species in rat bile which most likely classify as mono-oxo and di-oxo-taurocholates (MW 513 Da, 511 Da) and mono-oxo-glycocholates (MW 463 Da). In the present study we show that using this system it is possible to determine both conjugated and unconjugated as well as sulfated bile acids, without time consuming group separation and derivatization, from rat bile and human serum. In addition, it is suggested that the method presented here should be considered for use in routine analysis.
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  • 84
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Sugars ; Amperometric detection ; Chemically modified electrodes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A chemically modified electrode was applied as a working electrode for the amperometric detection of sugars in liquid chromatography. A mixture of cuprous oxide and conductive carbon cement was used as electrode material. Cuprous oxide acted as a catalyst for the oxidation of sugars. Cyclic voltammetry was used to examine the oxidation of the sugars at the electrode surface. The stability and sensitivity of a cuprous oxide/conductive carbon cement (20/80 %, w/w) electrode were tested in flow injection analysis experiments. For liquid chromatography, sugars were separated on an ion-exclusion column with 0.01 M H2SO4 as mobile phase. After the separation, 0.2 M NaOH was added post-column and the sugars were determined at 550 mV vs. Ag/AgCl. Calibration was linear in the range of 10−6·10−3 M with limits of detection of approximately 1·10−6M. The application of the modified electrode for the determination of sugars in fruit beverages and dairy products following chromatographic separation is shown.
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  • 85
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Structure vs. retention ; Principal component analysis ; Multiple linear regression ; Molecular descriptors
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The mechanism of the retention in HPLC when using a non-polar solvent with a very low content of polar modifier as mobile phase is outside the scope of the classical interpretations. We have used quantitative structure-retention relationships (QSRR) to interpret the retention of a series of 36 compounds on 18 chromatographic systems (3 stationary phases and 6 mobile phases). Principal Component Analysis (PCA) was used to reduce the complexity of the data and to obtain the most significant axis; molecular modeling (molecular mechanics and molecular orbital calculations) was used to obtain structural information on the solutes, and multiple regression to correlate coordinates and descriptors. We have shown that the coordinates of the solutes on the first PCA axis are related to three molecular descriptors: the calculated logarithm of the partition coefficient in an octanol/water system (Log P), the polarisability (pol) and the energetic level of the highest occupied molecular orbital (HOMO). We have found the same equation with a similar coefficient for the three different stationary phases. These results prove the dominant role of the polar modifier in such chromatographic systems.
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  • 86
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    Chromatographia 40 (1995), S. 129-133 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Digalactosyldiacylglycerols ; Solid phase extraction ; Oats ; Experimental design
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A convenient method for the isolation of digalactosyldiacylglycerols from plant material has been developed using solid phase extraction. Commerical cartridges were utilized to prepare 100 mg fractions of galactolipids containing more than 97% of digalactosyldiacylglycerol. The purity of the fractions was monitored by an isocratic normal phase analytical HPLC procedure, which was optimized using factorial design. The optimized system was successfully scaled up to a semi-preparative HPLC system with a capacity of about 10 mg/injection which was used to further purify the digalactosyldiacylglycerol fraction.
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  • 87
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Electrospray ionization mass spectrometry ; Micropellicular poly-styrene/divinylbenzene ; Peptides and proteins
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Short columns packed with highly crosslinked 2.3 μm poly-styrene/divinylbenzene (PS/DVB) particles were used for rapid and efficient separation of proteins and peptides by reversed-phase high-performance liquid chromatography at elevated temperatures. Enhancement of the diffusivities of the sample components at elevated temperatures together with the short diffusion pathlength with the micropellicular polymeric stationary phases were responsible for high efficiency, high speed of analysis, and short column regeneration times. Underivatized PS/DVB beads as well as PS/DVB microspheres which have been modified with polyvinylalcohol or octadecyl chains on the surface were synthesized, employed, and compared to HY-TACH-C18, a commercially available micropellicular octadecyl-silica stationary phase, for the separation of proteins, octapeptides and tryptic protein digests. Highest performance was obtained with the silica- and PS/DVB-based octadecyl stationary phases, which exhibited similar column efficiencies but different selectivities for proteins and peptides. The minimum detectability at 214 nm and the maximum loading capacity for ribonuclease A using analytical 30×4.6 mm I.D. columns were 10 ng (0.6 pmol) and 1 μg, respectively. Finally, reversed-phase HPLC with a 60×2 mm I.D. narrow-bore column packed with micropellicular octadecyl PS/DVB was coupled successfully to electrospray mass spectrometry at a flow-rate of 0.15 mL min−1 and on-line full-scan mass spectra for molecular mass determination and identification of proteins in the lower picomol range were obtained.
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  • 88
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Benzalkonium chloride ; Tramadol ; Ophthalmic solution
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A high-performance liquid chromatographic procedure employing ultraviolet detection for the analysis of benzalkonium chloride in 0.5% Tramadol ophthalmic solution is reported. The method requires minimal sample pretreatment and is sensitive, accurate, and reproducible. The peak area versus BAK concentration is linear over the range of 50–150% of its label claim of 0.05 mg/mL. The mean absolute recovery of BAK using the described method is 100.2±1.2%, (mean ±SD, n=10). A stress study with heat, acid, base and UV radiation indicates that the method is stabilityindicating with no interference from drug or degradation products.
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  • 89
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Fluorescence enhancement ; Bovine serum albumin ; Dansylamino acids
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The effects of acetonitrile and bovine serum albumin (BSA) concentrations on the signal intensity and retention behavior of dansylamino acids have been examined by using γ-cyclodextrin-bonded silica gel as the stationary phase in microcolumn liquid chromatography. Fluorescence intensities of dansylamino acids were enhanced by BSA as a mobile phase additive, e.g., detection limits of dansyl derivatives of L-Ala and L-Phe were improved by a factor of 12–18.
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  • 90
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Isoniazid in milk ; SPE preconcentration ; Diode array UV spectra
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A simple, fast, accurate and highly sensitive (5 ng/ml) method for the detection of sionicotinic acid hydrazide (isoniazid) in cattle milk is described, based upon an RP-HPLC system, equipped with a C18 column and a UV detector. Milk was deproteinized with trichloroacetic acid and treated with cinnamaldehyde, before being injected into the HPLC system. Preconcentration of samples on an SPE phenyl cartridge allows the sensitivity of the method to be increased to 0.05 ng/ml using a UV detector. The presence of isoniazid can be confirmed at concentrations as low as 0.4 ng/ml, through a diode-array UV spectrum of isoniazid hydrazone. The analytical procedure here described is routinely applied to investigate the illegal administration of isoniazid to cattle, as it provides a means of screening that can be carried out in a very short time.
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  • 91
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Micellar liquid phases ; Octanol-water partition coefficient ; Benzene and naphthalene derivatives
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary It is shown that the logarithm of the capacity factor (log k′) for fifteen benzene and naphthalene derivatives in micellar liquid chromatography with forty nine different mobile phases generally correlates better with the logarithm of the octanol-water partition coefficient (log Pow) than the capacity factor (k′). Optimum conditions are established to obtain the best linear correlations of log k′-log Pow.
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  • 92
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    Chromatographia 40 (1995), S. 193-196 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chemometric methodology ; Elution order ; Simplex optimization ; Benzodiazepines
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Using a rapid chemometric methodology to determine the separation factor, α, at different temperatures, Gibbs Helmholtz parameters (Δ (ΔH), Δ (ΔS), Δ (ΔG)) of two adjacent benodiazepines on a chromatogram were obtained from ln α versus T−1 plots. A temperature dependent reversal of the elution order was studied and the mobile phase composition and column temperature were optimized to obtain the best separation. A flow rate of 0.80 ml min−1 with 52.6% methanol in the methanol-water mixture and a column temperature of 48°C gave the most efficient separation of ten benzodiazepines.
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  • 93
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    Chromatographia 40 (1995), S. 204-206 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Stability-indicating method ; 17β-Estradiol-3-phosphate ; Ophthalmic solutions
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A reversed-phase high-performance liquid chromatographic (HPLC) procedure using ultra-violet (UV) detection for the analysis of 17β-estradiol-3-phosphate in an ophthalmic solution is reported. The method is selective, accurate, and reproducible. The peak area versus 17β-estradiol-3-phosphate concentration is linear over the range of 50–150% of its label claim of 1.0 mg/mL, with a detection limit of 20 ng/mL. The mean absolute recovery of 17β-estradiol-3-phosphate using the described method is 99.8±0.6% (mean ±SD, n=10). A stress study with heat, acid, base and UV radiation indicates that the method is stability-indicating with no interference from excipients or degradation products.
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  • 94
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Photolysis ; Electrochemical detection ; Drugs with chlorinated aromatic rings
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Pharmaceuticals containing a thiazide ring or chlorinated aromatic ring were investigated with respect to enhanced selectivity in determination. Oxidative electrochemical detection coupled with HPLC was used to study the influence of the pH of the mobile phase under conditions of photolysis. To cover a pH range 3.9–12, the employment of a polymer column stable in alkaline media was necessary. The method offers the great advantage of derivatization without chemicals at low operating potentials, thereby providing high selectivity.
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  • 95
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    Chromatographia 40 (1995), S. 237-246 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Mixed mode stationary phases ; Indirect photometric and fluorometric detection ; Conductimetric detection ; Alkyl-sulphates, and sulphonat-phosphates
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Separation of three classes of anionic surfactants (alkyl sulfates, alkanesulfonates, and alkyl phosphates) are achieved on a mixed-mode reversed phase (RP) phenyl/-anion exchange column using a naphthalenetrisulfonate (NTS)-acetonitrile (ACN) mobile phase via indirect photometric, indirect fluorometric, direct or indirect conductivity detection. Mixtures of C5−C18 sulfates, C6−C18 sulfonates, and C1−C4 phosphates (mono- and di-ester) can be separated in less than 20, 24, and 20 min respectively. Although hydrophobic effects are more pronounced in mixed-mode chromatography, equivalent-per-equivalent exchange of analysis and eluent ion is still required for sensitive indirect photometric, fluorometric, or conductivity detection. The detection limits of alkyl sulfates and alkanesulfonates are in the range of 3–15 pmoles which are at least an order of magnitude better than suppressed conductivity detection. The determination of surfactants in a variety of real samples is also presented.
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  • 96
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Reversed phase ; Polystyrene ; Pellicular ; Ultra high molecular mass
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Ultra high molecular mass (〉 7 million dalton) polystyrenes are prone to degradation in size exclusion chromatography. In gradient elution reversed phase HPLC they do not elute visibly on small particle size porous supports. However, large diameter C18 pellicular particles were successfully employed for reversed phase study of ultra high molecular mass (15 million dalton) polystyrenes without polymer degradation during elution. Although retention for the lower molecular mass polystyrenes was lower than on small diameter porous particles, the medium high molecular mass polystyrenes (0.5–1 million dalton) showed similar retention. The addition of small diameter porous particles in small quantities, to the large diameter pellicular particles, increased the amount of retention of the low molecular mass polystyrenes without affecting the higher molecular mass polystyrenes.
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  • 97
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Multicomponent mobile phases ; Retention prediction ; Binary and multicomponent phases, comparison
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Using the concept of an effective concentration a method is proposed for predicting retention in liquid chromatography with multicomponent mobile phases based on experiments with corresponding binary ones. The method is verified for normal and reversed-phase systems with ternary mobile phases and agrees closely with experimental data.
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  • 98
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Methyl ethyl ketone in urine ; Derivatization ; 3-Methyl-2-benzothiazolinone hydrazone ; Comparison with GC-MS
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A HPLC method for the determination of methyl ethyl ketone (MEK) in urine after derivatization with 3-methyl-2-benzothiazolinone hydrazone is proposed. The calibration curve for the ketone was linear, ranging between 0.23–10 mg/L, with a detection limit of 0.025 mg/L. The results were compared to those obtained by GC-MS, coupled to the headspace technique. MEK derivatization and the derivative purification processes were verified with respect to the main variables such as reaction temperature, reagent concentration, probable interferences and enrichment phase. The method is simple and reliable and shows a good sensitivity.
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  • 99
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Indirect photometric detection ; Anthraquinone-disulfonate ion ; Inorganic anions
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Disodium salts of several anthraquinone-disulfonic acids, which possess large molar absorptivity, were employed as the visualization agent for microcolumn ion chromatography with indirect photometric detection. Detection limits of inorganic anions were improved, e.g., concentration detection limits of chloride, nitrate and sulfate were 0.91–1.6 μmol L−1 at S/N=3, corresponding to mass detection limits of 18–32 fmol. The present system was applied to the determination of inorganic anions in tap water.
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  • 100
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    Chromatographia 40 (1995), S. 382-386 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Sulfonamides in foodstuffs ; Honey ; Milk ; Eggs
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A procedure for the simultaneous determination of several sulfonamides in different foods, such as honey, milk and eggs is proposed. The analysis is carried out using reversed phase liquid chromatography with spectrophotometric detection. Optimization of the mobile phase led to good separation and a short analysis time when an initial isocratic step with a 3∶97 acetonitrile: water mixture was used for 5 minutes, followed by a linear gradient up to a 40∶60 mixture over 15 min. The proposed method is suitable for routine quality control analysis to ensure the absence of sulfonamides in foods. Recovery studies yielded good results for all food samples because there were no interferences from the matrices.
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