Improved determination of alkanolamines by liquid chromatography with electrochemical detection

doi:10.1016/S0021-9673(01)93036-5

Journal of Chromatography A

Volume 546, 1991, Pages 381-385

https://doi.org/10.1016/S0021-9673(01)93036-5 Get rights and content

Abstract

The determination of alkanolamines has traditionally been difficult due to the complexity of the detection methods and the difficulty of the separation. Wet chemistry, gas chromatography and high-performance liquid chromatography methods all required time-consuming, complex sample treatments which are prone to numerous interferences.

This paper will describe the use of a liquid chromatography method using a polymer based reversed-phase column coupled to a pulsed amperometric detector. This method provides simple, direct quantitation of triethanolamine. Evaluation of this method for linearity, reproducibility and detection limits in an alkaline etch process will be presented.

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Determination of biogenic amines in alcoholic beverages by ion chromatography with suppressed conductivity detection and integrated pulsed amperometric detection
2007, Journal of Chromatography A
The determination of biogenic amines in alcoholic beverages is important to assess the potential risks associated with the consumption of high concentrations of these compounds. In addition, product storage conditions and the length of storage can cause the formation of biogenic amines that reduce product quality. We report a new method using cation-exchange chromatography with either suppressed conductivity, integrated pulsed amperometry, UV, or a combination of these detection techniques to determine biogenic amines in alcoholic beverages. The main objective was to provide a direct comparison between IPAD and suppressed conductivity detection for determining biogenic amines in alcoholic beverages. Suppressed conductivity is the simplest detection approach for determining putrescine, cadaverine, histamine, agmatine, phenylethylamine, spermidine, and spermine with good sensitivity (0.004–0.08 mg/l) and was used to evaluate the influence of storage time and conditions on the evolution of biogenic amines in alcoholic beverages. Integrated pulsed amperometric detection (IPAD) detects more biogenic amines than suppressed conductivity detection, enabling the detection of dopamine, tyramine, and serotonin. Tyramine was simultaneously determined by UV detection and IPAD to provide confirmation and ensure the accuracy of the analytical results. The linearity of biogenic amine responses was within 0.1–20 mg/l and peak area precisions were 0.24–4.97% for IPAD, suppressed conductivity-IPAD, and UV detection. The sensitivity for the 10 biogenic amines using the 3 detection techniques varied considerably from 0.004–1.1 mg/l and recoveries were within 85–122%.
Improved ion chromatography-integrated pulsed amperometric detection method for the evaluation of biogenic amines in food of vegetable or animal origin and in fermented foods
1998, Journal of Chromatography A
An improved method for the simultaneous determination of underivatized biogenic amines, cadaverine, putrescine, spermidine, histamine, tyramine and some amino acids precursors, histidine and tyrosine, in food products, based on ion-exchange chromatography (IC) with integrated pulsed amperometric detection (IPAD) has been developed. The method was successfully used for the analysis of biogenic amines and amino acids in food both of vegetable (kiwi, Actinidia chinensis) and animal origin, (fish, pilchard), as well as in fermented foods, such as cheese (Emmenthal) and dry sausages (salami). The method was also successfully used to study the changes in biogenic amines during the ripening of dry fermented sausages (salami). The analytes were extracted from foods with perchloric acid and the extracts were purified by liquid–liquid partition using n-hexane. Determination of biogenic amines was performed through cation-exchange chromatography with isocratic elution and IPAD. The detection limits for the analytes under investigation were found to range from 1.25 to 2.50 ng, at a signal-to-noise ratio of 3:1. Average recoveries ranged from 85.5 to 97.4% and R.S.D. values ranged from 3.4 to 8.8. The proposed method offers a number of advantages over our previous IPAD method, such as the application to a larger number of analytes and matrices, a simpler extraction procedure and clean-up, isocratic elution using low acid and base concentrations, an improved chromatographic separation and a lower detection limit.
Pulsed electrochemical detection of alkanolamines separated by multimodal high-performance liquid chromatography
1995, Journal of Chromatography A
Pulsed electrochemical detection (PED) is applied to alkanolamines separated by high-performance liquid chromatography (HPLC). A multimodal HPLC column with both cation-exchange and reversed-phase retention modes is used with an acidic mobile phase to assure alkanolamines are in their cationic form. Baseline resolution of alkanolamines, including positional isomers, is possible. Detector response for a representative alkanolamine, tris(hydroxymethyl)aminomethane (Tris), is shown to be linear over a concentration range of more than three decades. The limit of detection for Tris is 20 nM (500 fmol in a 25-μl injection) and the standard deviation of the PED response for 10 μM Tris is better than 0.4%. HPLC-PED is demonstrated to permit the sensitive and precise determination of alkanolamines in a biological sample (blood) and a commercial formulation (shaving gel) with minimal sample preparation.
Pulsed Electrochemical Detection of Carbohydrates at Gold Electrodes Following Liquid Chromatographic Separation
1995, Journal of Chromatography Library
This chapter describes pulsed electrochemical detection (PED) of carbohydrates at gold (Au) electrodes following liquid chromatographic separation. PED technology has been developed to achieve the highly sensitive and reproducible detection of alditols, monosaccharides, and oligosaccharides at Au electrodes. Sensitivity of PED at Au electrodes is maximized under conditions of high alkalinity, and pH > 12 is commonly recommended. Whereas all carbohydrates yield a PED response, only aldoses (reducing sugars) can be detected selectively as a result of the judicious choice of detection potential within PED waveforms. The analytic impact of liquid chromatography (LC)-PED can be appreciated on the basis of the recognition that (1) carbohydrates are polar compounds and, therefore, are not easily separated by gas chromatography and (2) these compounds are aliphatic without conjugated bonding and, therefore, are not easily detected by conventional photometric or fluorometric techniques without a priori derivatizations to attach chromophoric functional groups. In addition, the use of pellicular polymeric ion-exchange phases has been most popular to achieve separations in LC-PED because their stability at pH extremes is most consistent with use of highly alkaline mobile phases required for maximum sensitivity in PED at Au electrodes.
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Improved determination of alkanolamines by liquid chromatography with electrochemical detection

Abstract

Anal. Chim. Acta

Update Report: The Determination of Alkanolamine Scrubbers by ion Chromatography

Gulf Coast Conference, Houston, TX