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气相色谱-质谱联用分析布托啡诺的衍生化方法

Derivatization methodology for the analysis of butorphanol by gas chromatography-mass spectrometry.

作者信息

Andraus M H, de Siqueira M E

机构信息

Antidoping Laboratory of Jockey Club de São Paulo, Brazil.

出版信息

Biomed Chromatogr. 1998 Jan-Feb;12(1):34-7. doi: 10.1002/(SICI)1099-0801(199801/02)12:1<34::AID-BMC718>3.0.CO;2-D.

Abstract

Butorphanol is an opioid used as analgesic in humans and other species. In horses, it can cause locomotor stimulation at low doses. This drug is not well chromatographed by GC and so, it is necessary to transform it into a more suitable compound, which can be done by derivatization. The derivatization of a drug is used to impart volatility, masking polar groups to improve the results in gas chromatographic analysis. We have evaluated N,O-bis(trimethylsilyl)- trifluoracetamide (BSTFA)+ 1% trimethylchlorsilane (TMCS) and N-methyl-N-trimethylsilil-trifluoroacetamide (MSTFA) as derivatizing reagents for butorphanol at 30, 60 and 80 degrees C during 15, 30 and 60 min. The effects of dilution of these reagents with toluene and the evaporation before the derivatization were tested. Both reagents can be used for butorphanol derivatization and analysis and the dilution and evaporation steps did not alter the final results. The best derivatization conditions were 15 min at 80 degrees C, although 60 degrees C, although 60 degrees C during 60 min were also suitable.

摘要

布托啡诺是一种在人类和其他物种中用作镇痛药的阿片类药物。在马中,低剂量时它会引起运动刺激。这种药物用气相色谱法(GC)色谱分析效果不佳,因此,有必要将其转化为更合适的化合物,这可以通过衍生化来实现。药物的衍生化用于赋予挥发性,掩盖极性基团以改善气相色谱分析结果。我们评估了N,O-双(三甲基硅基)-三氟乙酰胺(BSTFA)+1%三甲基氯硅烷(TMCS)和N-甲基-N-三甲基硅基-三氟乙酰胺(MSTFA)作为布托啡诺在30、60和80摄氏度下15、30和60分钟的衍生化试剂。测试了这些试剂用甲苯稀释以及衍生化前蒸发的效果。两种试剂均可用于布托啡诺的衍生化和分析,稀释和蒸发步骤不会改变最终结果。最佳衍生化条件是在80摄氏度下15分钟,不过在60摄氏度下60分钟也合适。

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