高效液相色谱-串联质谱法检测绿茶中硝苯地平

Determination of Nifedipine in Green Tea by HPLC-MS/MS

风险监测显示市面上陆续出现了添加硝苯地平等二氢吡啶类降血压药物的绿茶,而我国目前尚未有绿茶中硝苯地平的权威检测方法。本试验根据实际需要建立了液相色谱串联质谱法检测绿茶中硝苯地平的方法。首先对绿茶样品进行前处理,采用甲醇超声提取,经过CARB-NH2固相萃取柱净化;然后进行色谱分析,以Inertsil ODS-3(150 mm×2.1 mm,5.0μm)为液相色谱柱,乙腈、0.2%乙酸水溶液为流动相,流速为0.3 mL/min;质谱采用正离子扫描,多反应监测方式检测绿茶中的硝苯地平含量。试验考察了方法学中的线性方程、检出限和定量限、加标回收率、重复性等指标。结果表明:在1~20 ng/mL范围内线性良好,相关系数为0.9996;检出限为13.8μg/kg,定量限为46.0μg/kg;加标回收率在2、4、8 ng/mL三个水平分别为83.5%、86.3%、89.6%,相应水平重复性依次为3.98%、3.43%、1.16%;所考察的指标均满足方法学要求。该方法操作简单、准确、可行,适用于绿茶中硝苯地平的检测。

Risk monitoring shows that green tea with dihydropyridine antihypertensive drugs such as nifedipine appears on the market in succession.However,there is no authoritative method for the determination of nifedipine in green tea in China.According to the actual needs,a method using HPLC-MS/MS for the determination of nifedipine in green tea was established.The pretreatment method of CARB-NH2 solid phase extraction column purification after utrasonic extraction of green tea samples with methanol was established.The method was developed based on novel HPLC column Inertsil ODS-3(150 mm×2.1 mm,5.0μm)with acetonitrile,0.2%acetic acid as mobile phase,with flow rate at 0.3 mL/min.Methods positive ion scanning and multi reaction monitoring were used to detect nifedipine residues in green tea.The linear equation,limit of detection and limit of quantification,recovery of standard addition,repeatability and other indexes in methodology were investigated.The results show that in the range of 1-20 ng/mL,r=0.9996,detection limit was 13.8μg/kg,limit of quantitation was 46.0μg/kg,the recoveries were 83.5%,86.3% and 89.6% at 2,4,8 ng/mL levels,and the repeatability was 3.98%,3.43% and 1.16% respectively.All the indexes meet the requirements of methodology,and the method is simple,accurate and feasible,suitable for the determination of nifedipine in green tea.