液质联用法检测中成药和保健食品中添加辅助降血糖类药品的研究

目的: 建立准确、灵敏的HPLC-MS/MS方法,检测中药制剂及保健食品中非法添加11种辅助降血糖类化学药物。方法: 样品经甲醇提取后,采用液相色谱/电喷雾离子化质谱法测定。色谱条件:Ultimate XB-C₁₈(2.1 mm×150 mm,3.5 μm),柱温30 ℃,流动相以甲醇-0.1%乙酸铵溶液进行梯度洗脱,流速0.2 mL·min^-1;质谱条件:以电喷雾电离源正离子模式进行质谱数据采集。结果: 在上述色谱及质谱条件下,11种辅助降血糖类化学药物的HPLC色谱图分离度良好,质谱分辨率符合鉴别要求。HPLC-MS/MS方法测定上述化学物质的最小检出量为0.01~1.4 mg·kg^-1。结论: 该方法简便、快捷,灵敏度、准确性、重现性均可满足定性检查的要求。

Objective: To develop an HPLC-electrospray ion trap mass spectrometry method for identifying eleven kinds of auxiliary hypoglycemic agents in traditional Chinese medicine preparations and healthy foods. Methods: The liquid chromatography-electrospray ion trap mass spectrometry method was used to detect the samples extracted with methanol.The HPLC chromatographic determinations were run on an Waters HPLC/MSD trap using Ultimate XB-C₁₈(2.1 mm×150 mm,5 μm)column.The column temperature was 30 ℃.The mobile phase were grading of 0.1% ammonium acetate solution and methanol at a flow rate of 0.2 mL·min^-1.The mass spectrometer conditions were as follows:The fragmentation pattern of these drugs was analyzed by the mass spectrometer after being separated by HPLC,operated in positive ion. Results: A good resolution of eleven kinds of auxiliary hypoglycemic agents were obtained by HPLC and MS.The determination limits were in the range of 0.01-1.4 mg·kg^-1. Conclusion: The method is simple,rapid,sensitive and accurate.