液相色谱-串联高分辨质谱法测定动物源性食品中去氢表雄酮残留量
王舒婷，李嘉，程用斌，吴晓红，张婷，凌莉
陕西省农业检验检测中心，西安 710003
Determination of dehydroepiandrosterone residues in animal derived foods by liquid chromatography tandem high resolution mass spectrometry
-WANG Shuting, LI Jia, CHENG Yongbin, WU Xiaohong, ZHANG Ting, LING Li
Agricultural Inspection and Testing Center of Shaanxi province, Xi'an 710003, China
摘要：建立超高效液相色谱-四级杆-静电场轨道阱串联质谱法测定动物源性食品（包括猪肉、牛肉 、羊肉、鸡肉和鸭肉）中去氢表雄酮残留量。采用 Hypersil GOLD-C18 色谱柱为分析柱，以 0.1%（体积分数）甲酸溶液-甲醇作为流动相，梯度洗脱分离干扰物质，在电喷雾正离子模式下，用平行反应监测扫描模式采集数据，利用保留时间和相对离子丰度进行双重定性，基质匹配内标法定量。 去氢表雄酮的质量浓度在 2～250 ng/mL 范围内线性关系良好，相关系数为0.999 9，方法检出限为 2.0 ?g/kg，定量限为 4.0 ?g/kg。 在 4.0、8.0、10.0 ?g/kg 3 个添加水平下平均回收率为 85.4%～100.3%，测定结果的相对标准偏差为 1.9%～6.8% （n=5）。 该法可以快速、高效测定动物源性食品中去氢表雄酮残留量，为体育赛事运动员专供动物源性食品中去氢表雄酮残留量检测提供方法和技术。
Abstract：A method for the determination of dehydroepiandrosterone in animal derived foods including pork, beef, lamb, chicken and duck by ultra high performance liquid chromatography-tandem high resolution mass spectrometry was established. Hypersil GOLD-C18 chromatographic column was used as the analysis column, 0.1% (volume fraction) formic acid solution-methanol was used as the mobile phase, the interfering substances was separated by gradient elution. The target object was detected by electrospray ionization mass spectrometry in the positive ion mode with parallel reaction monitoring (PRM) scan mode. Retention time and relative ion abundance were used for dual qualitative analysis, and matrix matching internal standard method was used for quantification. The mass concentration of dehydroepiandrosterone had a good linear relationship in the range of 2-250 ng/mL, with the correlation coefficient of 0.999 9. The detection limit of the method was 2.0 μg/kg, and the quantitative limit was 4.0 μ g/kg. The average recoveries at spiked levels of 4.0, 8.0 and 10.0 μg/kg were 85.4%-100.3%, and the relative standard deviations of the determination results were 1.9%-6.8% (n=5). The method can be used to determine the amount of dehydroepiandrosterone residues in animal derived foods quickly and efficiently, which provides the techniques for the detection of dehydroepiandrosterone residues in animal derived foods specifically provided for athletes in sports events.
关键词：去氢表雄酮；食源性兴奋剂；高分辨质谱仪
Keywords：dehydroepiandrosterone; foodborne stimulants; high resolution mass spectrometer
本文引用格式：
王舒婷，李嘉，程用斌，等.液相色谱-串联高分辨质谱法测定动物源性食品中去氢表雄酮残留量[J].化学分析计量，2023，32
(10)：66.WANG Shuting，LI Jia，CHENG Yongbin，et al. Determination of dehydroepiandrosterone residues in animal derived foods by liquidchromatography-tandem high resolution mass spectrometry[J]. Chemical Analysis and Meterage，2023，32(10)：66.
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