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尿液中克伦特罗的气相色谱-质谱分析

Gas chromatography-mass spectrometric analysis of clenbuterol from urine.

作者信息

Keskin S, Ozer D, Temizer A

机构信息

Turkish Doping Control Center, Hacettepe University, Ankara.

出版信息

J Pharm Biomed Anal. 1998 Dec;18(4-5):639-44. doi: 10.1016/s0731-7085(98)00284-2.

DOI:10.1016/s0731-7085(98)00284-2
PMID:9919964
Abstract

Clenbuterol which is mostly used as an anabolic agent. It is also used for treatment of asthma. Clenbuterol was analysed from urine by using gas chromatography-mass spectrometry. GC-MS parameters were determined. Timolol was used as an internal standard. Extraction and derivatisation procedure of clenbuterol from urine were developed. Clenbuterol was extracted by using diethylether/ter-butanol (4:1; v:v) and pH 12 K2CO3/KHCO3 (3:2; w:w) buffer. MSTFA/NH4I (1 ml/10 mg) mixture was used for derivatization of clenbuterol. Selected ions of clenbuterol-bis-TMS were m/z: 405, 337, 336, 335, 300, and 227. Extraction yield and minimum detection limit of clenbuterol from urine were identified. Extraction yield was 94.30% and minimum detection was found 0.02 ng ml(-1) urine. It has been concluded that the GC-MS method is sensitive, accurate, precise, and reproducible for analysing of clenbuterol from urine.

摘要

克伦特罗主要用作合成代谢剂,也用于治疗哮喘。采用气相色谱-质谱联用仪从尿液中分析克伦特罗,确定了气相色谱-质谱联用仪的参数,使用噻吗洛尔作为内标。建立了从尿液中提取和衍生化克伦特罗的方法。采用乙醚/叔丁醇(4:1;v:v)和pH 12的碳酸钾/碳酸氢钾(3:2;w:w)缓冲液提取克伦特罗,使用MSTFA/NH4I(1 ml/10 mg)混合物对克伦特罗进行衍生化。克伦特罗-双三甲基硅基的选择离子为m/z:405、337、336、335、300和227。确定了尿液中克伦特罗的提取率和最低检测限,提取率为94.30%,最低检测限为0.02 ng/ml尿液。得出结论,气相色谱-质谱联用方法对尿液中克伦特罗的分析具有灵敏、准确、精密和可重现性。

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