GC-MS and HPLC-FLD for sensitive assay of toxic cyclohexylamine in artificial sweetener tablets and human biological fluids

IF 3.9 3区医学 Q2 FOOD SCIENCE & TECHNOLOGY

Food and Chemical Toxicology Pub Date : 2025-04-11 DOI:10.1016/j.fct.2025.115447

Hazim M. Ali , Amr A. Essawy , Ahmed Hamad Alanazi , Arafa Musa , Ahmed Emad F. Abbas , Ibrahim Bayoumi Abdel-Farid , Mohammed Gamal

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Abstract

Cyclohexylamine (CHA) is a precursor in the synthesis of artificial sweeteners cyclamate and its major metabolite. CHA is toxic to the nervous system, kidneys, and liver in animal studies. In the present work, gas chromatography-mass spectrometry (GC-MS) and high-performance liquid chromatography-fluorescence detection (HPLC-FLD) were introduced for the first time to the determination of nano-level concentration of CHA in artificial sweetener tablets and human biological fluids. According to the obtained results, HPLC-FLD and GC-MS of CHA exhibit a wide linear range from 1 to 1250 ng/mL and 5–1500 ng/mL within limits of detection of 0.49 and 1.55 ng/mL, respectively. Furthermore, both chromatographic techniques exhibited high accuracy and precision, yielding recovery estimates ranging from 95.85 % to 100.70 % for the HPLC-FLD method and 91.54 %–99.64 % for the other while the corresponding values of relative standard deviation (RSD%) range from 0.25 to 0.82 % and 1.25–3.97 %. The accuracies for HPLC-FLD and GC-MS method in serum and urine samples are within the range of 90.29–99.94 %. On the other hand, CHA was detected in all studied artificial sweetener tablets, its level ranged from 1.35 to 102.64 ng/tablet. Also, the results obtained from the HPLC-FLD and GC-MS methods were statistically compared, and no significant difference was found.

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GC-MS和HPLC-FLD对人工甜味剂片剂和人体生物体液中有毒环己胺的灵敏测定

环己胺（CHA）是合成人造甜味剂环己胺素及其主要代谢物的前体。在动物实验中，CHA对神经系统、肾脏和肝脏都是有毒的。本文首次将气相色谱-质谱联用（GC-MS）和高效液相色谱-荧光检测（HPLC-FLD）技术应用于人工甜味剂片剂和人体生物体液中CHA的纳米浓度测定。结果表明，CHA的HPLC-FLD和GC-MS在1 ~ 1250 ng/mL和5 ~ 1500 ng/mL范围内呈较宽的线性关系，检出限分别为0.49和1.55 ng/mL。两种色谱技术均具有较高的准确度和精密度，回收率分别为95.85% ~ 100.70%和91.54% ~ 99.64%，相对标准偏差（RSD%）分别为0.25% ~ 0.82%和1.25% ~ 3.97%。HPLC-FLD法和GC-MS法测定血清和尿液样品的准确度在90.29 ~ 99.94%之间。另一方面，在所有研究的人工甜味剂片剂中均检测到CHA，其含量范围为1.35 ~ 102.64 ng/片。HPLC-FLD法与GC-MS法测定结果进行统计学比较，差异无统计学意义。

本文章由计算机程序翻译，如有差异，请以英文原文为准。

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来源期刊

Food and Chemical Toxicology 工程技术-毒理学

CiteScore

10.90

自引率

4.70%

发文量

651

审稿时长

31 days

期刊介绍： Food and Chemical Toxicology (FCT), an internationally renowned journal, that publishes original research articles and reviews on toxic effects, in animals and humans, of natural or synthetic chemicals occurring in the human environment with particular emphasis on food, drugs, and chemicals, including agricultural and industrial safety, and consumer product safety. Areas such as safety evaluation of novel foods and ingredients, biotechnologically-derived products, and nanomaterials are included in the scope of the journal. FCT also encourages submission of papers on inter-relationships between nutrition and toxicology and on in vitro techniques, particularly those fostering the 3 Rs. The principal aim of the journal is to publish high impact, scholarly work and to serve as a multidisciplinary forum for research in toxicology. Papers submitted will be judged on the basis of scientific originality and contribution to the field, quality and subject matter. Studies should address at least one of the following: -Adverse physiological/biochemical, or pathological changes induced by specific defined substances -New techniques for assessing potential toxicity, including molecular biology -Mechanisms underlying toxic phenomena -Toxicological examinations of specific chemicals or consumer products, both those showing adverse effects and those demonstrating safety, that meet current standards of scientific acceptability. Authors must clearly and briefly identify what novel toxic effect (s) or toxic mechanism (s) of the chemical are being reported and what their significance is in the abstract. Furthermore, sufficient doses should be included in order to provide information on NOAEL/LOAEL values.