超高效液相色谱-串联质谱法同时测定保健食品中15种非法添加降糖化学药物

Simultaneous determination of 15 kinds of illegally added hypoglycemic chemicals in health foods by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  保健食品  降糖化学药物  非法添加

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  health food  hypoglycemic chemical  illegally added

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)同时测定保健食品中15种非法添加降糖化学药物的方法。方法 样品采用乙腈超声提取, 采用UPLC-MS/MS进行检测, 以Atlantis?dC15 (2.1 mm×150 mm, 3 μm)为色谱柱, 0.1%甲酸水溶液(A)-乙腈(B)为流动相, 梯度洗脱程序为0~3 min, 90%A; 3~15min, 90%~60%A; 15~28 min, 60%~0%A; 28~29 min, 0%A; 29~30 min, 0~90%A; 30~31 min, 90%A); 体积流量0.3 mL/min, 柱温40 ℃, 进样体积5 μL。选择ESI离子源, 多反应监测模式(multiple reaction monitoring, MRM), 通过比较MRM通道中样品峰与对照品峰的分子离子峰, 二级碎片离子峰等信息确定添加的化学药。结果 15种化学药物的线性范围宽, 相关性好, r≥0.995, 相对标准偏差(relative standard deviation, RSD)为1.58%~5.12%(n=6); 加标浓度为20、100、200 ng/mL时, 回收率为81.0%~120.1%,检出限为0.010~0.120 μg/g, 定量限在0.034~0.39 μg/g。应用该方法对48批样品进行了检测, 其中有2批次样品中检出盐酸苯乙双胍和格列本脲。结论 本方法专属性强, 灵敏度高, 适合用于保健食品中非法添加15种降糖化学药物的快速检测。

英文摘要:

      Objective To establish a method for simultaneous determination of 15 kinds of illegally added hypoglycemic chemicals in health foods by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The sample was ultrasonically extracted with acetonitrile and detected by UPLC-MS/MS, using Atlantis?dC15 (2.1 mm × 150 mm, 3 μm) as the column and 0.1% aqueous formic acid (A)-acetonitrile (B) as mobile phase. The gradient elution program was 0-3 min, 90%A; 3-15min, 90%-60%A; 15-28 min, 60%-0%A; 28-29 min, 0%A; 29-30 min, 0~90%A; 30-31 min, 90%A. The volume flow rate was 0.3 mL/min, the column temperature was 40 ℃, and the injection volume was 5 μL. Results The linear range of 15 chemical drugs was wide and the correlation was good, r≥0.995, and the relative standard deviation (RSD) was 1.58%-5.12% (n=6). The recoveries at 3 spiked (20, 100, 200 ng/mL) were 81.0%-120.1%, the limits of detection were 0.010-0.120 μg/g, and the limits of quantification were 0.034-0.39 μg/g. The 48 batches of samples were tested by this method, and phenformin hydrochloride and glibenclamide were detected in 2 batches. Conclusion This method has strong specificity and high sensitivity, which is suitable for rapid detection of illegally adding 15 kinds of hypoglycemic chemicals in health foods.