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目的:利用液相色谱-串联质谱联用仪,建立食品和饲料中醋酸甲孕酮的检测方法,并用来调查醋酸甲孕酮在食品和饲料中的污染情况。方法:样品加醋酸缓冲溶液均质,加酶溶液酶解后,再加甲醇超声提取。用叔丁基甲醚萃取2次,萃取液经反相固相萃取柱净化;以乙腈-水为流动相,经反相C18柱分离后进行LC/MS/MS分析。质谱采用正离子扫描模式,离子源为ESI(+),定量检测方式为多反应监测(MRM)方式,利用保留时间和碎片信号比值判断定性结果。结果:醋酸甲孕酮线性相关系数r为0.9983,变异系数在1.1%~5.8%之间,高、中、低不同水平的加标回收率在85.9%~97.2%之间。检测了56份肉类食品和13份饲料样品,结果显示食品中未检出醋酸甲孕酮,饲料中有3份检出少量的醋酸甲孕酮,含量在0.21~0.91μg/kg之间。结论:该方法简便快速,精密度较高,重现性较好,可应用于食品和饲料中醋酸甲孕酮的测定。饲料中检出少量的醋酸甲孕酮有待进一步确证和寻找来源。
OBJECTIVE: To establish a method for the determination of medroxyprogesterone acetate in food and feed by liquid chromatography-tandem mass spectrometry and to investigate the contamination of medroxyprogesterone acetate in food and feed. Methods: The sample was homogenized with acetic acid buffer solution and enzymatically hydrolyzed with enzyme solution, then extracted with methanol. The reaction mixture was extracted twice with tert-butyl methyl ether. The extract was purified by reverse-phase solid-phase extraction (SPE). The mobile phase was acetonitrile-water and separated by reversed-phase C18 column and analyzed by LC / MS / MS. The mass spectrometry was performed in positive ion scan mode with ESI (+) ion source and multiple reaction monitoring (MRM) as quantitative detection method. The qualitative results were judged by the ratio of retention time and debris signal. Results: The linear correlation coefficient (r) of medroxyprogesterone acetate was 0.9983, the coefficient of variation was between 1.1% and 5.8%, and the spike recoveries were between 85.9% and 97.2% at different levels of high, medium and low. 56 meat products and 13 feed samples were tested. The results showed that no medroxyprogesterone acetate was detected in the food, and 3 of the feed samples detected a small amount of medroxyprogesterone acetate in the range of 0.21-0.91 μg / kg. Conclusion: The method is simple, rapid, accurate and reproducible. It can be applied to the determination of medroxyprogesterone acetate in food and feed. Detection of a small amount of feed medroxyprogesterone acetate needs further confirmation and find the source.