气相色谱-质谱法初筛和确证运动营养品中甲基己胺  

Screening and Confirmation of Methylhexanamine in Sports Supplements through Gas Chromatography-Mass Spectrometry

作　　者：王占良[1] 张建丽[1] 张亦农[1] 

机构地区：[1]国家体育总局反兴奋剂中心食品药品兴奋剂检测实验室,北京100029

出　　处：《中国运动医学杂志》2014年第10期1004-1008,共5页Chinese Journal of Sports Medicine

摘　　要：目的：建立气相色谱-质谱法初筛和确证运动营养品中甲基己胺快速检测方法。方法：样品采用甲醇超声提取。弱阳离子交换固相萃取柱（MCX）纯化，洗脱液再经过液液萃取提取，30℃下氮气吹干，N-甲基-N-（三甲基硅烷）三氟乙酰胺衍生化后，采用HP-1MS柱（17m×0．2mmi．d．×0．11mm）色谱分离，程序升温，质谱检测。结果：甲基己胺的差向异构体在确证分析中实现基线分离，3个定性特征离子的峰度比计算结果满足世界反兴奋剂机构（WADA）要求。该方法的检测限为100μg／kg，在添加的高、中、低3种浓度的相对回收率分布在75％～120％，满足常规检测要求，样品前处理简单、快速、可靠。Objective To screen and confirm methylhexanamine in sports supplements through gas chromatography-mass spectrometry. Methods The sample was extracted by methanol and purified by MCX Oasis solid prepared extraction column,the elution was extracted by methyl tert-butyl ether,the methylhexanamine was completely separated by HP-1MS column （17 m × 0.2 mm i.d. × 0.11 p,m thickness）in linear temperature program. Results The epimers of methylhexanamine was separated in baseline and the calculated results of three characteristic ions in methylhexanamine accorded to the requirement of WADA technical documents. The relative recovery of methylhexanamine spiked in blank sample at high,middle and low level concentration ranged from 75 to 120%. The limit of detection for target analytes was 100 μg/kg. Conclusion The method introduced here is simple,rapid,reliable and suitable for analysis of Moutine in sports supplements.

关 键 词：甲基己胺 兴奋剂 运动营养品 气相色谱-质谱法(GC/MS) 

分 类 号：TS218[轻工技术与工程—粮食、油脂及植物蛋白工程] O657.63[轻工技术与工程—食品科学与工程]