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气相色谱/质谱法测定毛发中的β2-激动剂

Determination of beta 2-agonists in hair by gas chromatography/mass spectrometry.

作者信息

Polettini A, Montagna M, Segura J, de la Torre X

机构信息

Laboratory of Forensic Toxicology, University of Pavia, Italy.

出版信息

J Mass Spectrom. 1996 Jan;31(1):47-54. doi: 10.1002/(SICI)1096-9888(199601)31:1<47::AID-JMS248>3.0.CO;2-O.

Abstract

A method is described for the determination of the beta 2-agonists clenbuterol and salbutamol in hair. The method involves washing hair in sodium dodecyl hydrogensulphate solution, chemical digestion of the hair matrix in alkaline medium, solid-phase extraction, derivatization with methylboronic acid and analysis by gas chromatography/electron impact mass spectrometry in either the selected-ion monitoring or the scan mode. the effects of chemical digestion and of extraction on the recovery of the analytes were evaluated. Derivatization with methyl-boronic acid was compared with trimethylsilylation for GC/MS analysis of hair extracts, and was found to give mass spectra which showed more structural information with less chemical noise and better sensitivity. The proposed method was tested on real hair samples obtained from guinea pigs treated with growth-promoting doses of clenbuterol and salbutamol. Both compounds could be detected in hair of treated animals.

摘要

描述了一种测定毛发中β2-激动剂克伦特罗和沙丁胺醇的方法。该方法包括在十二烷基硫酸氢钠溶液中清洗毛发,在碱性介质中对毛发基质进行化学消解,固相萃取,用甲基硼酸衍生化,并通过气相色谱/电子轰击质谱在选择离子监测或扫描模式下进行分析。评估了化学消解和萃取对分析物回收率的影响。将用甲基硼酸衍生化与用三甲基硅烷化进行毛发提取物的气相色谱/质谱分析进行了比较,发现前者给出的质谱显示出更多的结构信息,化学噪声更少且灵敏度更高。用从接受促生长剂量克伦特罗和沙丁胺醇治疗的豚鼠获得的真实毛发样本对所提出的方法进行了测试。在接受治疗动物的毛发中均可检测到这两种化合物。

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