超高效液相色谱-串联质谱法测定红曲类保健品中的桔青霉素

Determination of Citrinin in Red Yeast Rice Healthcare Products by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了高效液相色谱-串联质谱对红曲类保健品中的桔青霉素含量进行检测的方法。采用70%甲醇-水溶液提取样品,经HLB固相萃取小柱净化后,通过高效液相色谱-串联质谱法测定桔青霉素的含量,多反应监测(MRM)方式监测离子对m/z 251→233(桔青霉素)外标法定量。结果表明,桔青霉素基质曲线在浓度5~100 ng/mL范围内线性关系良好(R^(2)=0.999),精密度RSD为2.8%,方法的定量限为37.5μg/kg,平均回收率在85.9%~87.8%的范围内。该方法快速、灵敏、结果准确,比液相方法操作简便,成本低,更适用于基质复杂的保健品中桔青霉素的定性定量检测。

In this study we established a determination method for citrinin in red yeast rice healthcare products by high performance liquid chromatography-tandem mass spectrometry.70%methanol-water solution was used to extract the sample.After purification with an HLB solid-phase extraction column,the content of citrinin was determined by high performance liquid chromatography-tandem mass spectrometry.The ion pair m/z 251→233(citrinin)was selected for multiple reaction monitoring(MRM),and the external standard method was adopted for quantification.The citrinin matrix curve had a good linear relationship in the concentration range of 5 ng/mL to 100 ng/mL(R^(2)=0.999),the precision RSD was 2.8%,the limit of quantification of the method was 37.5μg/kg,and the average recovery was in the range of 85.9%to 87.8%.The method is fast,sensitive,and accurate.It is cheaper and simpler to operate than the liquid phase method,and is more suitable for the qualitative and quantitative analysis of citrinin in healthcare products with complex matrix.