Therapeutic monitoring of antituberculosis drugs by direct in-line extraction on a high-performance liquid chromatography system

doi:10.1016/0378-4347(93)80118-N

Journal of Chromatography B: Biomedical Sciences and Applications

Volume 619, Issue 2, 22 September 1993, Pages 285-290

https://doi.org/10.1016/0378-4347(93)80118-N Get rights and content

Abstract

A direct in-line pre-column extraction technique in which guanidinium and ammonium sulfate are used, followed by column switching, was employed to analyze serum, plasma and cerebrospinal fluid samples of patients treated for tuberculous meningitis. Resolution of a wide range of polar to non-polar xenobiotics was obtained on a C₈ silica column by using a linear gradient from a binary system consisting of solvent A (0.05 M KH₂PO₄) and solvent B (acetonitrile—isopropanol, 4:1, v/v). Apart from the anti-tuberculosis drugs (isoniazid, pyrazinamide, ethionamide and rifampicin) the patients received up to sixteen different medicines for prevention of complications and the treatment of symptoms. Qualitative resolution of all the drugs was obtained by the chromatographic system. Quantitation of pyrazinamide and ethionamide was achieved with high precision and low inter-sample variation.

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Cited by (28)

Validation of a simple HPLC-UV method for rifampicin determination in plasma: Application to the study of rifampicin arteriovenous concentration gradient
2016, Journal of Pharmaceutical and Biomedical Analysis
Citation Excerpt :
Given this variability, therapeutic drug monitoring (TDM) of RFA is useful to overcome low plasma concentrations, therapeutic failure and prevent resistance or drug-related toxicity [3]. To that end, several analytical methods have been proposed for RFA determination in plasma [4–15]. In clinical practice, TDM of RFA and clinical PK investigations is performed using venous blood sampling in patients.
In clinical practice, rifampicin exposure is estimated from its concentration in venous blood samples. In this study, we hypothesized that differences in rifampicin concentration may exist between arterial and venous plasma.
An HPLC-UV method for determining rifampicin concentration in plasma using rifapentine as an internal standard was validated. The method, which requires a simple protein precipitation procedure as sample preparation, was performed to compare venous and arterial plasma kinetics after a single therapeutic dose of rifampicin (8.6 mg/kg i.v, infused over 30 min) in baboons (n = 3).
The method was linear from 0.1 to 40 μg mL⁻¹ and all validation parameters fulfilled the international requirements. In baboons, rifampicin concentration in arterial plasma was higher than in venous plasma. Arterial C_max was 2.1 ± 0.2 fold higher than venous C_max. The area under the curve (AUC) from 0 to 120 min was ∼80% higher in arterial plasma, indicating a significant arteriovenous concentration gradient in early rifampicin pharmacokinetics. Arterial and venous plasma concentrations obtained 6 h after rifampicin injection were not different.
An important arteriovenous equilibration delay for rifampicin pharmacokinetics is reported. Determination in venous plasma concentrations may considerably underestimate rifampicin exposure to organs during the distribution phase.
Electroanalysis of antitubercular drugs in pharmaceutical dosage forms and biological fluids: A review
2015, Analytica Chimica Acta
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Several analytical methodologies have been reported to determine antitubercular drugs. These include high performance liquid chromatography (HPLC) [12,13], HPLC assay employing solid phase extraction [14,15], liquid chromatography coupled with mass spectrometry [16,17], thin-layer chromatography [18,19], spectrofluorimetry [20], voltammetry [21,22], colorimetry [23], titrimetry [24], capillary zone electrophoresis [25], flow injection analysis (with the analyser having a photomultiplier tube detector) [26], and spectrophotometry [27]. Voltammetric techniques have proved to be a powerful and versatile method for the sensitive determination of drugs due to their extreme simplicity, low-cost instrumentation, relatively short analysis time, large linear dynamic range and high sensitivity, specificity, accuracy and precision compared to other analytical methods [28–30].
Tuberculosis remains a major global public health problem. Given the need for extensive analysis of antitubercular drugs, the development of sensitive, reliable and facile analytical methods to determine these compounds becomes necessary. Electrochemical techniques have inherent advantages over other well-established analytical methods, this review aiming to provide an updated overview of the latest trends (from 2006 till date) in the voltammetric determination of antitubercular drugs. Furthermore, the advantages and limitations of these methods are critically discussed. The review reveals that in spite of using a variety of chemically modified electrodes to determine antitubercular drugs, there is still a dearth of applicability of the voltammetric methods to quantify these compounds in human body fluids, especially in blood plasma.
Quantification of rifampicin in human plasma and cerebrospinal fluid by a highly sensitive and rapid liquid chromatographic-tandem mass spectrometric method
2012, Journal of Pharmaceutical and Biomedical Analysis
Citation Excerpt :
In all cases there are some drawbacks associated with existing methods making them unsuitable for satisfactory quantitative analysis in studies that have been designed and implemented as part of an integrated TB clinical pharmacology programme in the Liverpool School of Tropical Medicine. In some cases there is no inclusion of an IS which compromises the robustness of the method [8,15,17], some assays need relatively large volumes of sample and/or lacked sensitivity which limits their usefulness in pediatric studies where sample volumes are severely constrained [12–14] and other assays involve complex or very long extraction procedures thereby compromising throughput [10,11,13,16]. The aim of the work presented here was to develop a rapid and sensitive LC–MS/MS method for the quantification of RIF in human plasma and CSF samples.
A highly sensitive and rapid liquid chromatography tandem mass spectrometry (LC–MS/MS) method has been developed to measure the levels of the antitubercular drug rifampicin (RIF) in human plasma and cerebrospinal fluid (CSF). The analyte and internal standard (IS) were isolated from plasma and CSF by a simple organic solvent based precipitation of proteins followed by centrifugation. Detection was carried out by electrospray positive ionization mass spectrometry in the multiple-reaction monitoring (MRM) mode. The assay was linear in the concentration range 25–6400 ng/mL with intra- and inter-day precision of <7% and <8%, respectively. The validated method was applied to the study of RIF pharmacokinetics in human CSF and plasma over 25 h period after a 10 mg/kg oral dose.
A rapid and sensitive HPLC-MS method for the detection of plasma and cellular rifampicin
2007, Journal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences
Rifampicin is active against both intracellular and extracellular Mycobacterium tuberculosis. The ability to measure rifampicin drug concentrations in both plasma and in cells may be useful in evaluating the suitability of dosage regimens for populations and individuals. Here a novel simple, precise and accurate method for the quantification of rifampicin in both cells and plasma is reported. Sample proteins were precipitated with acetonitrile containing the internal standard and then diluted with water. Aliquots of supernatant were then injected into the HPLC–MS system for chromatographic separation and detection. Rifampicin calibration curves encompassed concentrations from 100 to 12,800 ng/mL. Intra- and inter-assay precision and accuracy were determined using low, medium and high concentration quality control samples and was found to be within 10% in all cases. Rifampicin concentrations were found to be unaffected by freeze–thaw cycles, but were significantly affected by heat-inactivation (58 °C, 40 min). This assay was successfully utilised to determine the pharmacokinetic profile of rifampicin in plasma and peripheral blood mononuclear cells (PBMC) in 8 tuberculosis patients receiving rifampicin over an 8 h period.
Therapeutic monitoring of anti-infectious drugs
2004, Revue Francaise des Laboratoires
Si la relation entre la pharmacocinétique et la pharmacodynamie (PK/PD) est clairement établie pour bon nombre d'antibiotiques, pour d'autres anti-infectieux, cette relation est aléatoire et il n'est pas possible d'établir des règles générales. Chaque médicament, chaque famille thérapeutique doit être considérée comme autant de cas particuliers. Parmi les paramètres utiles, la mesure de la concentration maximale est un indicateur d'efficacité pour les antibiotiques dont l'activité bactéricide augmente avec la concentration ou lorsque l'effet post-antibiotique est important et dépend de la dose. C'est le cas des aminosides et des fluoroquinolones dont l'activité bactéricide est concentration-dépendante. En revanche, les glycopeptides qui sont «temps-dépendants comme les tétracyclines ou le fluconazole, ne bénéficient que sous certaines conditions d'un suivi thérapeutique étroit. Quant aux bêta-lactamines, «temps-dépendantes leur suivi thérapeutique est dénué d'intérêt. Plus complexe est la conduite à tenir en matière d'antiviraux, d'antiparasitaires, d'antituberculeux et d'antifongiques. Nous présentons la relation PK/PD de certains agents anti-infectieux et l'intérêt que peut revêtir l'approche de leur pharmacocinétique pour optimiser le traitement des maladies sur lesquelles ils agissent.
If the relationship between pharmacokinetics and pharmacodynamics (PK/PD) is fairly established for many antibiotics, for others, this relationship is unclear. This is why it is not possible to set up general rules; each drug or at least each therapeutic family is to be considered as a particular case. Among parameters to be studied owing to plasma concentration measurements, peak concentration is the leading indicator for antibiotic efficacy insofar as bactericidal activity is increased with increasing drug concentration or when post-antibiotic effect is high and is dose-dependent. This is the case for aminoglycosides and fluoroquinolones with concentration-dependent activity. On the other hand, glycopeptides which are «time-dependant as tetracyclines or fluconazole, take only benefit from therapeutic drug monitoring under specific circumstances. As for beta-lactamines, which «time-dependent their therapeutic drug monitoring is senseless. More difficult are decisions to take in the case of antiviral drugs, antimalarials, anti-tuberculous drugs and antifungal agents. When present the PK/PD relationship of various anti-infectious agents and the interest of pharmacokinetics approach in order to optimize infectious diseases treatments.
Liquid chromatographic determination of isoniazid, pyrazinamide and rifampicin from pharmaceutical preparations and blood
2002, Journal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences
Isoniazid (IN), pyrazinamide (Pz) and rifampicin (Rf) are separated on YMC-ODS column. IN was derivatized with 2-fluorene-carboxaldehyde (FA). The separation was achieved using ethanol–chloroform–acetonitrile water by isocratic elution and detected at 337 nm. The detection limits were 0.11 ng, 0.2 ng and 13 ng/injection (5 μl) for IN, Pz and Rf, respectively. The method of analysis was applied to the pharmaceutical preparations and in the blood samples of the patients suffering from tuberculosis after undergoing chemotherapy with IN, Pz and Rf. The amounts quantitated in blood showed 0.97 to 1.58 μg/ml IN, 3.44 to 4.09 μg/ml Pz and 1.98 to 3.5 μg/ml Rf with coefficient of variations 0.8–1.8%, 0.9–1.3% and 0.8–2.1%, respectively.

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Therapeutic monitoring of antituberculosis drugs by direct in-line extraction on a high-performance liquid chromatography system

Abstract

J. Chromatogr.

J. Pediatr.

J. Chromatogr.

J. Chromatogr.

J. Chromatogr.