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采用基于多糖的手性柱-高分辨质谱法同时分析44种常见滥用皮质类固醇药物。

Simultaneous analysis of 44 frequently abused corticosteroid drugs using polysaccharide-based chiral column-HRMS approach.

作者信息

Karakka Kal Abdul Khader, Karatt Tajudheen K, Nalakath Jahfar, Subhahar Michael Benedict, Koshy Shino Ann, Perwad Zubair, M P Muhammed Ajeebsanu

机构信息

Equine Forensic Unit Central Veterinary Research Laboratory Dubai United Arab Emirates.

出版信息

Anal Sci Adv. 2021 Feb 19;2(9-10):427-439. doi: 10.1002/ansa.202000166. eCollection 2021 Oct.

DOI:10.1002/ansa.202000166
PMID:38716441
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC10989529/
Abstract

Corticoids have found their way into the globe of sports, due to their anti-inflammatory properties, and have often found to be added to dietary supplements for illegally improving the effectiveness of their products. Earlier studies describe the detection of corticoids in several matrices, but this can be an incessant and continuous process as long because the doping practices continue. In this study, we report a technique to verify concurrently 44 of the foremost commonly abused synthetic corticoids (including chiral analogs) in equine plasma supported chiral liquid chromatography-electrospray ionization mass spectrometry. Polysaccharide -cellulose-5 column was used for chromatographic separation with a gradient mode. The validation studies were also meted out by using equine plasma so as to judge the suitability of the strategy. Detection limits were determined between 0.01 and 0.05 ng/mL and therefore the limit of quantification was between 0.1 and 0.5 ng/mL. Recovery and matrix effect on the analytes was further assessed. Since the developed method was ready to separate the corticoids and to differentiate chiral analogs at very low levels (in picograms), this separation techniques may be employed for the determination (confirmatory analysis) of the corticoids in the forensic and anti-doping application.

摘要

由于具有抗炎特性,皮质类固醇已进入体育界,并且经常被添加到膳食补充剂中以非法提高其产品的功效。早期研究描述了在几种基质中检测皮质类固醇的情况,但只要兴奋剂使用行为持续,这可能就是一个持续不断的过程。在本研究中,我们报告了一种基于手性液相色谱 - 电喷雾电离质谱法同时验证马血浆中44种最常被滥用的合成皮质类固醇(包括手性类似物)的技术。使用多糖 - 纤维素 - 5柱以梯度模式进行色谱分离。还使用马血浆进行了验证研究,以评估该方法的适用性。测定的检测限在0.01至0.05 ng/mL之间,定量限在0.1至0.5 ng/mL之间。进一步评估了回收率和基质对分析物的影响。由于所开发的方法能够在极低水平(皮克级)分离皮质类固醇并区分手性类似物,因此这种分离技术可用于法医和反兴奋剂应用中皮质类固醇的测定(确证分析)。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9a9d/10989529/b770cc959da3/ANSA-2-427-g023.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9a9d/10989529/effd397ae9ac/ANSA-2-427-g038.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9a9d/10989529/76883c43d2b0/ANSA-2-427-g048.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9a9d/10989529/bd3c33703552/ANSA-2-427-g010.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9a9d/10989529/0d97610c6c84/ANSA-2-427-g025.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9a9d/10989529/c25aca294bad/ANSA-2-427-g036.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9a9d/10989529/b770cc959da3/ANSA-2-427-g023.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9a9d/10989529/effd397ae9ac/ANSA-2-427-g038.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9a9d/10989529/76883c43d2b0/ANSA-2-427-g048.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9a9d/10989529/bd3c33703552/ANSA-2-427-g010.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9a9d/10989529/0d97610c6c84/ANSA-2-427-g025.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9a9d/10989529/c25aca294bad/ANSA-2-427-g036.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9a9d/10989529/b770cc959da3/ANSA-2-427-g023.jpg

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本文引用的文献

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Separation of ephedrine and pseudoephedrine enantiomers using a polysaccharide-based chiral column: A normal phase liquid chromatography-high-resolution mass spectrometry approach.使用多糖基手性柱分离麻黄碱和伪麻黄碱对映体:正相液相色谱-高分辨率质谱法
Chirality. 2019 Aug;31(8):568-574. doi: 10.1002/chir.23104. Epub 2019 Jun 27.
3
Enantiomeric resolution, thermodynamic parameters, and modeling of clausenamidone and neoclausenamidone on polysaccharide-based chiral stationary phases.
基于多糖的手性固定相上氯苯酰胺酮和新氯苯酰胺酮的对映体拆分、热力学参数及建模
Chirality. 2019 Jun;31(6):423-433. doi: 10.1002/chir.23068. Epub 2019 Apr 24.
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Chiral separation of aliphatic primary amino alcohols as o-phthaldialdehyde/mercaptoethanol derivatives on polysaccharide-based chiral stationary phases.在多糖基手性固定相上对作为邻苯二甲醛/巯基乙醇衍生物的脂肪族伯氨基醇进行手性拆分。
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