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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(17 m×0.2 mm i.d.×0.11 mm)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 establish a rapid and sensitive method for the detection of methylhexylamine in sports nutrition by gas chromatography-mass spectrometry. Methods: The samples were extracted by methanol ultrasonic extraction and weak cation exchange column (MCX). The eluate was extracted by liquid-liquid extraction and dried under nitrogen at 30 ° C. N-methyl-N- (trimethylsilyl) Trifluoroacetamide was derivatized with HP-1MS column (17 m × 0.2 mm id × 0.11 mm). The temperature was programmed and detected by mass spectrometry. Results: Methahexanamine epimers were baseline-separated in the confirmatory analysis, and the kurtosis ratios of the three qualitatively characteristic ions were calculated to meet the requirements of the World Anti-Doping Agency (WADA). The detection limit of this method was 100μg / kg. The relative recoveries of the three concentrations were 75% ~ 120% at the high, medium and low concentrations, which satisfied the routine testing requirements. The sample pretreatment was simple, rapid and reliable.