柱前衍生化后的超高效超临界流体色谱-质谱法快速测定含丙二醇糖浆中的痕量乙二醇和二甘醇。

IF 3.8 2区 化学 Q1 BIOCHEMICAL RESEARCH METHODS Journal of Chromatography A Pub Date : 2024-10-10 DOI:10.1016/j.chroma.2024.465433
Si-Tong Zheng , Zi-Ying Wang , Zhen Liu , Yingxiang Du , Ling Cao , Sheng Tang , Hian Kee Lee , Yaozuo Yuan , Hai-Wei Shi
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引用次数: 0

摘要

乙二醇(EG)和二甘醇(DEG)是两种已知会导致多种人体健康问题的污染物,当摄入一定量时,它们会造成不良影响,如肾毒性、神经毒性甚至死亡。它们广泛存在于丙二醇中,而丙二醇通常用作药用糖浆的基质。本研究旨在开发一种用于评估市售儿科糖浆中 EG 和 DEG 含量的分析方法。本研究开发了一种快速、简单、可靠的超高效超临界流体色谱-电喷雾质谱(UHPSFC-ESI-MS)方法。这项工作包括对 UHPSFC-ESI-MS 的三种衍生试剂进行评估。最终选定苯甲酰氯为最佳衍生试剂。与未衍生化的方法相比,本方法高效、灵敏、快速地实现了 EG 和 DEG 的分离和检测,并在 7 分钟内完成了糖浆配方中 EG 和 DEG 的分析。EG和DEG在0.25-25.0 μg/mL浓度范围内的线性判定系数均大于0.999。EG 和 DEG 的检出限分别为 0.02 μg/mL 和 0.07 μg/mL,定量限分别为 0.09 μg/mL 和 0.25 μg/mL。DEG和EG的回收率分别为85.5%-108.1%和86.7%-117.2%。三种糖浆中基质效应的绝对值均小于 10%。同时,建立了气相色谱-氢火焰离子化检测方法,对分析结果进行交叉检验。在 10 个批次的糖浆配方中,两种方法都没有检测到 DEG。UHPSFC-ESI-MS 仅在三个批次中检测到 EG 的存在,且均未超过百万分之 90.23(ppm),两组结果的平均绝对误差为百万分之 5.95。所开发的 UHPSFC-ESI-MS 方法快速、简便、高效、灵敏、准确,适用于真正的糖浆配方中 EG 和 DEG 的测定。
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Rapid Determination of Trace Ethylene Glycol and Diethylene Glycol in Propylene Glycol-Contained Syrups by Ultrahigh-Performance Supercritical Fluid Chromatography-Mass Spectrometry after Precolumn Derivatization
Ethylene glycol (EG) and diethylene glycol (DEG) are two contaminants known to cause a variety of human health problems, when ingested in certain amounts, they can cause adverse effects such as nephrotoxicity, neurotoxicity and even death. They are widely found in propylene glycol, which is commonly used as a base for pharmaceutical syrups. The aim of this study was to develop an analytical method for the evaluation of EG and DEG in commercially available pediatric syrups. In this study, a fast, simple and reliable ultrahigh performance supercritical fluid chromatography-electrospray ionization-mass spectrometry (UHPSFC-ESI-MS) method was developed. The work involved the evaluation of three derivatization reagents for UHPSFC-ESI-MS. Benzoyl chloride was finally selected as the optimal derivatization reagent. Compared with an approach without derivatization, the present method achieved the separation and detection of EG and DEG efficiently, sensitively and rapidly, and analysis of EG and DEG in syrup formulations was realized within 7 min. The linear determination coefficients of EG and DEG in the concentration range of 0.25–25.0 μg/mL were greater than 0.999. The limits of detection for EG and DEG were 0.02 μg/mL and 0.07 μg/mL, respectively, and the limits of quantification were 0.09 μg/mL and 0.25 μg/mL, respectively. The recovery rates of DEG and EG ranged from 85.5%–108.1% and 86.7%–117.2%, respectively. The absolute values of the matrix effects in the three types of syrups considered were all less than 10%. Meanwhile, a gas chromatography-hydrogen flame ionization detection method was established for cross-testing of the analytical results. In 10 batches of syrup formulations, DEG was not detected by either method. The presence of EG was detected by UHPSFC-ESI-MS in only three batches, none of which exceeded 90.23 parts per million (ppm), with a mean absolute error of 5.95 ppm between the two sets of results. The developed UHPSFC-ESI-MS method was rapid, simple, efficient, sensitive and accurate for the determination of EG and DEG in genuine syrup formulations.
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来源期刊
Journal of Chromatography A
Journal of Chromatography A 化学-分析化学
CiteScore
7.90
自引率
14.60%
发文量
742
审稿时长
45 days
期刊介绍: The Journal of Chromatography A provides a forum for the publication of original research and critical reviews on all aspects of fundamental and applied separation science. The scope of the journal includes chromatography and related techniques, electromigration techniques (e.g. electrophoresis, electrochromatography), hyphenated and other multi-dimensional techniques, sample preparation, and detection methods such as mass spectrometry. Contributions consist mainly of research papers dealing with the theory of separation methods, instrumental developments and analytical and preparative applications of general interest.
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