UPLC-MS法测定降压类中成药和保健食品中非法添加硝苯地平的含量

Content Determination of Nifedipine Illegally Added in Antihypertensive Chinese Patent Drug and Health Food by UPLC-MS

目的:建立UPLC-MS法测定降压类中成药和保健品中非法添加硝苯地平的含量。方法:采用ACQUITYUPLCr CSHTC181.7μm色谱柱(2.1mm×100mm);以乙腈-0.1%甲酸溶液(10:90)为流动相,梯度洗脱(0~5min,10%→99%乙腈,5~5.1min,10%乙腈,5.1~7min,10%乙腈),流速为0.3ml.min^(-1),进样量:1μl;正离子方式检测,扫描方式为多反应监测(MRM)。结果:硝苯地平质量浓度在4.04ng.ml^(-1)~404ng.ml^(-1)范围内与峰面积呈良好的线性关系(r=0.9997,n=6),平均回收率为98.99%,RSD=0.4%。结论:本方法快速、简单、精确、灵敏,可有效监测中成药和保健品中非法添加的硝苯地平。

Objective：To establish the content determination of nifedipine illegally added in antihypertensive Chinese patent drug and health food by UPLC-MS. Methods：Using theACQUITY UPLCr CSHT C 18 1.7 μm column （2.1 mm ×100mm ）;using acetonitrile and 0.1%formic acid solution（10：90） as the mobile phase, gradient elution （0-5min,10%→99% acetonitrile; 5.0- 5.1min, 10% acetonitrile, 5.1 - 7min,10% acetonitrile）, the flow rate was 0.3ml.min, injection volume： 1μl; positive ion detection mode; scanning method for multiple reaction monitoring（MRM）.Results： Nifedipine concentration of 3.162ng.ml-1 - 316.2ng.ml-1 range and peak area had a good linear relationship （r=0.9997, n=6）, the average recovery was 98.99%, RSD=0.59%. Conclusion： This method is simple, accurate, reliable, sensitive and Can effectively monitor the nifedipine illegal｜y added in antihypertensive Chinese patent drug and health food.