UPLC-DAD Q TOF MS/MS法快速检测降血压类保健食品及中成药中添加的20个化学药物  

Rapid determination of twenty added chemicals in anti-hypertensive Chinese traditional medicine and health foods by UPLC-DAD-Q-TOF-MS/MS

作　　者：赵琪 贾昌平 钱叶飞 陈卫 张超 ZHAO Qi;JIA Chang-ping;QIAN Ye-fei;CHEN Wei;ZHANG Chao(Suzhou Institute for Drug Control,Suzhou 215000,China)

机构地区：[1]苏州市药品检验检测研究中心,苏州215000

出　　处：《药物分析杂志》2024年第6期990-998,共9页Chinese Journal of Pharmaceutical Analysis

基　　金：江苏省药品监督管理局科研计划课题(编号202128)。

摘　　要：目的:利用超高效液相-串联四极杆-飞行时间液质(UPLC-DAD Q TOF MS/MS)联用系统,建立快速可靠灵敏的测定降压类保健食品及中成药中违法添加阿奇沙坦、硝苯地平、拉西地平、奈比洛尔等20个化学药物的液质联用检测方法。方法:采用UPLC-DAD-Q-TOF-MS/MS联用仪,以Waters HSS T3 C18(100 mm×2.1 mm, 1.8μm)为色谱柱,以0.1%甲酸水溶液(A)和甲醇-乙腈(1∶1)(B)为流动相,梯度洗脱(0 min, 5%A;0~8 min, 5%A→95%A;8~11 min, 95%A;11~11.2 min, 95%A→5%A;11.2~12 min, 5%),流速为0.3 mL·min^(-1);进样体积1μL;ESI正、负离子模式,一级、二级质谱全扫描,进行UPLC-DAD-Q-TOF-MS/MS的定性及定量分析。结果:经方法学验证,本方法在1~50μg·mL^(-1)浓度范围内线性良好、精密度(RSD)小于3%、回收率在80.5%~98.7%。应用该方法在15批样品中均含有非法添加的药物成分,其中14批样品检出2个及以上多种药物成分;9批样品均检出托拉塞米、坎地沙坦酯、拉西地平;另有一批样品检出乐卡地平和奈比洛尔,在降压类保健食品及中成药产品中首次检出。结论:本方法快速、准确,灵敏度高,在涵盖12个补充检验标准中的成分的基础上扩大了检验范围,为快速筛查降血压类保健食品及中成药中非法添加化学药物提供有力技术支撑。Objective:To establish a fast,accurate and sensitive method by UPLC-DAD-Q-TOF-MS/MS for the detection of 20 kinds of illegally added chemicals such as azilsartan,nifedipin,lacidipine、nebivolo in anti-hypertensive health foods.Methods:Waters HSS T3 C18(100 mm×2.1 mm,1.8μm)column was used with mobile phase of 0.01 mol·L^(-1)ammonium acetate aqueous solution-methanol and gradient elution(0 min,5%A;0-8 min,5%A→95%A;8-11 min,95%A;11-11.2 min,95%A→5%A;11.2-12 min,5%).The flow rate was 0.3 mL·min^(-1).The injection volume was 1μL.ESI+,ESI-scan and MS/MS mode were applied.Qualitative and quantitative analyses were carried out by UPLC-DAD-Q-TOF-MS/MS.Results:The method was validated.A good linear relationship was showed in the concentration of 1-50μg·mL^(-1),(RSD<3%)and the recovery was obtained in range of 80.5%-98.7%.Illegally added chemical drugs were found in 15 batches of samples tested by this method.Two or more types of drugs were detected in 14 batches of samples.Torsemide,candesartan cilexetil,lacidipine were detected in 9 samples.Lacidipine and nebivolol were found in one of the sample.Conclusion:This method is fast,accurate and sensitive with a high degree of separation.It can be used as a powerful tool for the fast detection of illegally added chemicals in anti-hypertensive health foods.

关 键 词：超高效液相-串联四极杆-飞行时间液质联用仪 降血压 非法添加化学药物 食品 中成药 乐卡地平 奈比洛尔 

分 类 号：R917[医药卫生—药物分析学]