高效液相色谱-串联质谱法同时测定蜂胶中31种酚类化合物  

Simultaneous determination of 31 phenolic compounds in propolis by highperformance liquid chromatography-tandem mass spectrometry

作　　者：张研 曹翠玲 祖铁红 李学民 李阿丹[1] 崔宗岩 ZHANG Yan;CAO Cuiling;ZU Tiehong;LI Xuemin;LI Adan;CUI Zongyan(College of Environmental and Chemical Engineering,Yanshan University,Qinhuangdao 066004,China;Technology Center of Qinhuangdao Customs,Qinhuangdao 066004,China)

机构地区：[1]燕山大学环境与化学工程学院,秦皇岛066004 [2]秦皇岛海关技术中心,秦皇岛066004

出　　处：《分析试验室》2023年第6期775-783,共9页Chinese Journal of Analysis Laboratory

基　　金：海关总署科研项目(2019HK090);河北省自然科学基金面上项目(B2021203005)资助。

摘　　要：建立了高效液相色谱-串联质谱法检测杨树属蜂胶和酒神菊属蜂胶中31种酚类化合物。蜂胶原料或蜂胶乙醇提取物用85%(V/V)乙醇水提取,Atlantis T3色谱柱分离,以甲醇-0.1%(V/V)甲酸水为流动相进行梯度洗脱,电喷雾离子化(ESI),多反应监测(MRM)模式检测,外标法定量。31种目标物线性关系良好,相关系数(R2)均大于0.99。在质量浓度0.25, 0.5, 2.5 g/kg 3个添加水平下,方法的加标回收率为80.5%~109.6%,相对标准偏差(RSD)为0.2%~12%。该方法适用于蜂胶原料和蜂胶乙醇提取物中31种酚类化合物的检测,可以为蜂胶质量评价提供一定支撑。A high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method was developed for the simultaneous determination of 31 phenolic compounds in Poplar-type propolis and Baccharis propolis.Propolis raw materials or propolis ethanol extracts were extracted by 85%(V/V)ethanol water.The 31phenolic compounds were separated by an Atlantis T3 column and gradiently eluted using methanol-0.1%(V/V)formic acid water as mobile phase.The detection of phenolic compounds was performed through electrospray ionization(ESI)under multiple reactions monitoring(MRM)mode and quantified by an external standard calibration.The 31 target compounds had good linear relationships with the correlation coefficients(R~2)0.99.At three spiked levels of 0.25,0.5 and 2.5 g/kg,the average recoveries of all compounds were 80.5%-109.6%with the relative standard deviations(RSDs)of 0.2%-12%.The method is applicable for the determination of 31phenolic compounds in propolis raw materials and propolis ethanol extracts,and can provide technical supports for quality evaluation of propolis.

关 键 词：蜂胶 酚类化合物 高效液相色谱-串联质谱(HPLC-MS/MS) 

分 类 号：S896.6[农业科学—特种经济动物饲养]