摘要
建立QuEChERS前处理结合超高效液相色谱-串联质谱法检测药膳材料中非法添加二氢吡啶类降压药及其降解杂质(非洛地平、非洛地平杂质Ⅰ、尼莫地平、尼莫地平杂质Ⅰ、尼群地平、尼群地平杂质Ⅰ、尼索地平、尼索地平杂质Ⅰ、尼索地平杂质Ⅱ、硝苯地平、硝苯地平杂质Ⅰ、硝苯地平杂质Ⅱ)的方法。采用ACQUITY UPLCHSS T3(2.1 mm×100 mm,1.8μm)色谱柱,以含0.1%乙酸的0.01 mol/L乙酸铵溶液和甲醇、乙腈比例为25∶15的溶液为流动相,进行梯度洗脱,进样量为2μL,流速为0.25 m L/min;采用电喷雾离子源、多反应监测、正离子扫描模式检测。结果显示,12种化学成分在测定浓度范围内线性关系良好,相关系数r≥0.9966;精密度、稳定性良好;各化合物的回收率均在80.71%~102.89%,RSDs≤5.21%。该方法简便易行、快速准确、选择性好、灵敏度高,能降低假阴性风险,可用于药膳材料中非法添加二氢吡啶类降压药及其降解杂质的检测。
An analytical method based on QuEChERS pretreatment combined with ultra-high performance liquid chromatography-tandem mass spectrometry was developed for the determination of illegal addition of dihydropyridine antihypertensive drugs and their degradation impurities(Felodipine,Felodipine impurity Ⅰ,Nimodipine,Nimodipine impurity Ⅰ,Nitrendipine,Nitrendipine impurity Ⅰ,Nisodipine,Nisodipine impurity Ⅰ,Nisodipine impurity Ⅱ,Nifedipine,Nifedipine impurity Ⅰ,Nifedipine impurity Ⅱ)in medicinal and edible materials.Chromatographic separation was performed on a Waters ACQUITY UPLC HSS T3 column(2.1 mm×100 mm,1.8μm).The mobile phase consisted of 0.01 mol/L ammonium acetate solution containing 0.1%acetic acid(A)and methanol-acetonitrile(25∶15,v/v)(B),using gradient elution.The flow rate was 0.25 mL/min,and the injection volume was 2μL.Detection was performed using electrospray ionization(ESI).Positive electrospray ionization(ESI+)was performed in multiple reaction monitoring(MRM)mode.All analytes showed good linearity(r≥0.9966)within the tested ranges.The precision and stability of the method were satisfactory for the twelve chemical components.The average recoveries of all compounds ranged from 80.71%to 102.89%with relative standard deviations(RSDs)≤5.21%.The established method is simple,rapid,accurate,selective,and highly sensitive,and can be used for the detection of illegal addition of dihydropyridine antihypertensive drugs and their related substances in medicinal and edible materials.
作者
刘云
孟育航
刘美玲
李培
高翔
常海莹
LIU Yun;MENG Yuhang;LIU Meiling;LI Pei;GAO Xiang;CHANG Haiying(Xinxiang Institute for Food and Drug Control,Xinxiang Henan,453000,China;School of Chemical Engineering,Zhengzhou University)
出处
《质量安全与检验检测》
2025年第6期38-44,共7页
QUALITY SAFETY INSPECTION AND TESTING
基金
河南省市场监督管理局科技计划项目(HNSCJGK202493)。
