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目的:建立同时测定辅助降血压类保健食品中非法添加的多个钙通道阻滞剂药物的HPLC-MS联用法。方法:色谱柱为Inertsil ODS-SP(5μm,4.6 mm×250 mm),流动相为0.1%甲酸-20 mmol.L-1甲酸铵(pH=4.8)-乙腈-甲醇,梯度洗脱;流速为1.0 mL.min-1,柱温为25℃。本文采用电喷雾离子源,西布曲明和华法林钠作为正、负离子模式下的内标物,0.2 mL.min-1的分流流速进离子阱质谱,选择离子模式(SIR)下定量检测地尔硫卓(m/z 414.75)、维拉帕米(m/z 455.14)、尼卡地平(m/z480.03)、氨氯地平(m/z 408.79)、硝苯地平(m/z 346.17)、尼群地平(m/z 360.36)、尼莫地平(m/z 417.75)、尼索地平(m/z387.27)、非洛地平(m/z 382.72)、西尼地平(m/z 491.52)、拉西地平(m/z 455.70)结果:利用本文建立的HPLC-MS法进行检测,11种化合物都有良好的线性范围和相关性(0.029～20.0μg·mL-1,R2≥0.9910),最低检出限为7.50～73μg.kg-1;回收率为64.6%～109.0%。结论:本方法选择性高,重复性好,能准确、快速、简便地应用于保健食品中非法添加钙通道阻滞剂类药物的检测。
OBJECTIVE: To establish a HPLC-MS method for the simultaneous determination of multiple calcium channel blockers illegally added in supplementary hypotensive health food. Methods: The mobile phase consisted of Inertsil ODS-SP (5 μm, 4.6 mm × 250 mm) and mobile phase consisted of 0.1 mmol formic acid and 20 mmol·L -1 ammonium formate (pH = 4.8) 1.0 mL.min-1, the column temperature was 25 ℃. In this paper, electrospray ionization source, sibutramine and warfarin sodium were used as internal standard in positive and negative ion mode, the flow rate was set at 0.2 mL.min-1 into ion trap mass spectrometry, and the quantitative detection of diltiazem in selective ion mode (SIR) (m / z 414.75), verapamil (m / z 455.14), nicardipine (m / z 480.03), amlodipine (m / z 408.79), nifedipine (M / z 360.36), nimodipine (m / z 417.75), nisoldipine (m / z 387.27), felodipine (m / z 382.72), cilnidipine (m / z 491.52) Laxidipine (m / z 455.70) Results: All of the 11 compounds had good linear range and correlation (0.029-20.0μg · mL-1, R2≥0.9910) by HPLC-MS method. The lowest The detection limit was 7.50 ~ 73μg.kg-1; the recovery was 64.6% ~ 109.0%. Conclusion: The method has high selectivity and repeatability, and can be used accurately, rapidly and simply in the detection of illegally added calcium channel blockers in health foods.