超高效液相色谱-串联质谱法同时测定保健品中非法添加的降糖减脂和利尿类药物

Simultaneous determination of anti-diabetic, anti-lipemic and diuretic drugs illegally added in health products by ultra performanceliquid chromatography-tandem mass spectrometry

中文关键词:  超效液相色谱-串联质谱法  保健品  非法添加  药物  降糖  减脂  利尿

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  health products  illegal added  drugs  anti-diabetic  anti-lipemic  diuretic

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)同时测定保健品中非法添加的降糖减脂和利尿类药物的分析方法。方法 样品用甲醇-水溶液(50:50, V:V)经超声提取, 经C18色谱柱(50 mm×2.1 mm, 2.6 μm)分离, 以0.1%(V/V)甲酸-10 mmol/L乙酸铵水溶液和乙腈作为流动相, 进行梯度洗脱。在正电喷雾离子(positiveelectrospray ionization, ESI+)源采用多反应监测(multiple reaction monitoring,MRM)模式检测。结果 3类非法添加药物在1.0~50.0 ng/mL范围内(洛伐他汀羟酸钠盐为10~500 ng/mL)线性均良好, 相关系数(r2)均在0.99以上。3类非法添加的药物在0.1、0.5和1.0 μg/g 3水平(洛伐他汀羟酸钠盐的加标量为1.0、5.0和10.0 μg/g)下的加标回收率为77.15%~116.61%, 相对标准标准偏差(relative standard deviations, RSDs)均未超过10.65%(n=6)。结论 本方法简单、快速、可靠、灵敏度高, 可满足保健品市场的监管和检验需求。

英文摘要:

      Objective To establish an analytical method for the determination of anti-diabetic, anti-lipemic and diuretic drug compounds added in health products by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods Samples were extracted with methanol-water (50:50, V/V) under ultrasonic condition, and separated on C18 chromatographic column (50mm×2.1mm, 2.6 μm). Gradient elution was carried out with 0.1% (V/V) formic acid-10 mmol/L ammonium acetate solution and acetonitrile as mobile phase. The determination was conducted in positive electrospray ionization(ESI+) mode under multiple reaction monitoring (MRM) mode. Results The linearity of 3 kinds of illegally added drugs were good in the range of 1.0-50.0 ng/mL (10?500 ng/mL for lovastatin sodium salt), with the correlation coefficients (r2) all above 0.99.The recoveries of all the illegal drugs in health products were 77.15%?116.61% with the relative standard deviations (RSDs) no more than 10.65% (n=6) at 3spiked levels, 0.1, 0.5, 1.0 μg/g (1.0, 5.0, 10.0 μg/g for lovastatin sodium salt). Conclusion This method is specific, easy, fast, accuracy and sensitive, which can meet the needs of supervise and inspect the illegal added drugs in health products market.