液相色谱-电喷雾串联质谱法同时测定蜂胶保健品中的活性成分和降糖西药

Simultaneous Determination of Active Components and Anti-diabetic Drugs in Propolis Health Foods by Ultra Performance Liquid Chromatography Tandem Mass Spectrometry

采用超高效液相色谱-电喷雾串联四极杆质谱仪(UPLC-ESI-MS/MS)同时测定蜂胶保健品中14种活性成分和9种违禁降糖西药。蜂胶保健品样品用甲醇稀释,超声波提取,样品溶液经高速离心后过滤。使用ACQUITY UPLC C18反相柱(50 mm×2.1 mm,1.7μm);流动相为0.3%甲酸溶液和乙腈,在梯度条件下分析,目标分析物在多反应监测(MRM)模式下以保留时间和离子对(母离子和两个碎片离子)信息比较进行定性和定量分析。本方法的活性成分检出限(LOD)为0.7～42.0 mg/kg;定量限(LOQ)为2.2～140 mg/kg;活性成分的加标回收率为77.8%～113.6%;违禁降糖西药的LOD为0.1～0.9 mg/kg,LOQ为0.3～2.5 mg/kg;违禁降糖西药的平均回收率为79.3%～108.5%。本方法简便、有效、灵敏,为评价蜂胶保健品质量提供了新的检测方法。

A comprehensive analytical method based on ultra performance liquid chromatography tandem mass spectrometry（UPLC-MS/MS） was developed for the simultaneous determination of active components and anti-diabetic drugs in propolis health foods.The samples were extracted by ultrasound extraction with methanol.The insoluble residue of extract was removed by freeze-centrifuging.The analysis was performed on an ACQUITY UPLC C_18 column（50 mm ×1 mm,i.d.,1.7 μm） utilizing a gradient elution profile and a mobile phase of 0.3% formic acid in water and acetonitrile.The analytes were detected using an electro spray ionization tandem mass spectrometry with multiple reaction monitoring.Qualitative and quantitative analysis was based on the peak area of the parent ion and two fragment ions.The LOD and LOQ level for 14 active components ranged from 0.7 mg/kg to 42.0 mg/kg and 2.2 mg/kg to 140 mg/kg respectively,and recoveries were 77.8%-113.6%,with the intra-and inter-day precision less than 15%.The LOD and LOQ level for 9 anti-diabetics ranged from 0.1 mg/kg to 0.9 mg/kg and 0.3 mg/kg to 2.5 mg/kg respectively,and recoveries were 79.3%-108.5%,with the intra-and inter-day precision less than 15%.The method is simple and sensitive,and can be used for quality control of propolis.