UPLC-MS/MS法同时快速测定保健食品中10种降压类非法添加化学药

Simultaneous and Rapid Determination of 10 illegally Added Antihypertensive Chemicals in Health Food by UPLC-MS/MS

目的:建立同时测定保健食品中10种降压类非法添加化学药的UPLC-MS/MS快速检测方法。方法:液相采用ACQUITY UPLC®BEH C_(18)(2.1 mm×100 mm,1.7μm)柱,以超纯水(含0.1%甲酸)-乙腈(0.1%甲酸)为流动相,进行梯度洗脱,进样量2μL,流速0.3 mL·min^(-1),柱温30℃。质谱采用ESI,正、负离子多反应监测模式,进行定性分析和定量分析。结果:盐酸普萘洛尔、酒石酸美托洛尔、艾司洛尔、比索洛尔、坎地沙坦、厄贝沙坦、替米沙坦、氯沙坦、缬沙坦和吲达帕胺的分离度良好,线性范围内相关性均较好,R^(2)均大于0.9963;平均回收率为93%~118%;RSD为1.4%~4.9%(n=6);方法检出限为0.10~5.00μg·kg^(-1);方法定量限为0.30~15.00μg·kg^(-1);单次分析仅需12 min。结论:该方法操作便捷、检测时间短、灵敏度高、结果准确,适用于保健食品中10种降压类非法添加化学药的快速筛查及定量检测。

Objective:To establish a UPLC-MS/MS rapid detection method for simultaneously determining 10 illegally added chemical antihypertensive drugs in health foods.Method:ACQUITY UPLC®BEH C_(18)(2.1 mm×100 mm,1.7μm)column was used in the liquid phase with ultrapure water(containing 0.1%formic acid)-acetonitrile(0.1%formic acid)as the mobile phase for gradient elution,the injection volume was 2μL,flow rate was 0.3 mL·min^(-1),and column temperature was 30℃.The mass spectrometry was performed by ESI,positive/negative ion multiple reaction monitoring mode for qualitative and quantitative analysis.Result:The separation degree of propranolol,metoprolol,amlodipine,bisoprolol,candesartan,irbesartan,telmisartan,losartan,valsartan,and indapamide was good,and the linear range correlations were good,all R^(2)values were greater than 0.9963.The average recovery rate was 93%~118%.RSD was 1.4%~4.9%(n=6).The LOD was between 0.10~5.00μg·kg^(-1),and the LOQ was between 0.30~15.00μg·kg^(-1).A single analysis only requires 12 min.Conclusion:The method is simple to operate,has short detection time,high sensitivity,and accurate results,and it is suitable for the rapid screening and quantitative detection of 10 illegally added chemical antihypertensive drugs in health foods.