建立了液相色谱-三重四极杆质谱法同时测定植物茶饮料中13种降糖类药物含量的方法.样品经甲醇溶液超声提取10 min后,定容至10.0 mL,过0.22 μm有机相滤膜,所得滤液采用Angilent Zorbax-Eclipse Plus C18色谱柱分离,以不同体积比的乙腈和0.1％(体积分数)甲酸(含5 mmol/L乙酸铵)水溶液进行梯度洗脱,质谱检测采用电喷雾离子源(ESI+)模式和多反应监测(MRM)模式,外标法定量.结果表明,13种降糖类药物标准曲线的线性范围为0.2～10.0 ng/mL,定量限(LOQ)为2.0 µg/kg,按标准加入法进行样品加标回收测试,回收率范围为85.9％～97.5％,测定值的标准偏差均≤5.87％.
Determination of 13 Kinds of Hypoglycemic Drugs in Plant Beverages by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry
A liquid chromatography-tandem mass spectrometry method has been developed for the simultaneous determination of 13 hypoglycemic drugs in plant beverages.The analytes in samples were extracted with methanol for 10 minutes by ultrasonic extraction.The target components were separated by an Angilent Zorbax Eclipse Plus C18 chromatographic column,and the gradient elution was carried out with different volume ratios of acetonitrile and 0.1％(volume fraction)formic acid(containing 5 mmol/L ammonium acetate)aqueous solution.The electrospray ionization in positive ion mode was used for analysis in multiple reaction moni-toring(MRM)mode,and an external standard method was used for quantitative analysis.The result showed that the linear range of the standard curves for 13 hypoglycemic drugs were 0.2-10.0 ng/mL,with a limit of quantification(LOQ)of 2.0 μg/kg.Standard addition method was used for sample recovery testing,with a recovery rate range of 85.9％-97.5％.The standard deviation of the measured values were less than 5.87％.
万方数据
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