超高效液相-三重四级杆质谱法测定健脾丸中展青霉素的含量

Determination of patulin in Jianpi Pills by ultra high performance liquid chromatography-tandem triple quadruple mass spectrometry

目的建立超高效液相-三重四级杆质谱法(UPLC-MS/MS)测定健脾丸中展青霉素的含量。方法样品经果胶酶酶解后,用乙酸乙酯提取展青霉素,提取液经HLB固相萃取小柱净化后,采用UPLC-MS/MS进行测定。结果展青霉素在0.020~2.010μg/ml内线性关系良好,回归方程为Y=666825X+27524(r=0.9970),检出限(LOD)为0.0101μg/ml,定量限(LOQ)为0.0201μg/ml。结论本法灵敏、快速、准确、专属性强,可用于健脾丸中展青霉素的测定。

Objective To establish an ultra high performance liquid chromatography-tandem triple quadruple mass spectrometry(UPLC-MS/MS)method for the content determination of patulin in Jianpi Pills.Methods After being enzyme-hydrolyzed by pectinase,extracted by water,and purified by HLB solid-phase extraction column,patulin were analyzed by UPLC-MS/MS.Results The calibration curves of the patulin showed good linearities in the range of 0.020-2.010μg/ml with the regression equation Y=666825X+27524(r=0.9970).The limit of detection(LOD)was 0.101μg/ml,and the limit of quantification(LOQ)was 0.0201μg/ml.Conclusion The method is sensitive,rapid,accurate and specific enough to determine patulin in Jianpi Pills.