浓缩石榴汁中熊果苷的超高效液相-串联质谱检测方法研究  

Study on detection method of arbutin in pomegranate juice concentrates by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：何强 孔祥虹 李建华 乐爱山 吴双民 

机构地区：[1]陕西出入境检验检疫局检验检疫技术中心,陕西西安710068

出　　处：《食品工业科技》2012年第10期62-65,共4页Science and Technology of Food Industry

基　　金：陕西省农业攻关项目(2010K01-19-4);国家质检总局科研项目(2009IK285);陕西出入境检验检疫局科研项目(2010IK001)

摘　　要：建立了浓缩石榴汁样品中熊果苷含量测定的固相萃取-超高效液相-串联质谱测定方法。样品用水稀释,HLB和氨基固相萃取柱净化,采用BEHAmide色谱柱(100mm×2.1mm,1.7μm)分离,以乙腈和水梯度洗脱,多反应监测模式测定,定量离子对为m/z271.2>108.0,定性离子对为m/z271.2>160.9,外标法定量。熊果苷的检测限为0.006mg/kg,在0.004～0.2mg/L浓度范围内,熊果苷的线性相关系数为0.9994,熊果苷的加标回收率均在80.6%～108.1%范围内,相对标准偏差均低于8.3%。该方法样品净化效果良好,检测简便、快速、准确,能够满足浓缩石榴汁中熊果苷含量测定和定性确证的要求。A method was developed for the determination of arbutin in pomegranate juice concentrate by solid phase extraction（SPE）and ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）.Samples were diluted by water and then cleanup with HLB and aminopropyl SPE columns.UPLC was performed on a BEH Amide column（100mm×2.1mm,1.7μm）using a gradient acetonitrile-water system as mobile phase,and MS/MS was performed with multiple reation monitoring（MRM）mode using m/z 271.2108.0 as quantitative ion pair and m/z 271.2160.9 as qualitative ion pair.Quantitation was carried out using an external standard method.The detection limit of arbutin was 0.006mg/kg and the calibration curves were linear at the range of 0.004～0.2mg/L with linear correlation coefficient as 0.9994.The recoveries ranged from 80.6% to 108.1% with relative standard deviations less than 8.3%.The results of sample cleanup were well,and the determination method was simple,fast and sufficient.It was suitable for quantitative and qualitative analysis of arbutin in pomegranate juice concentrate.

关 键 词：浓缩石榴汁 熊果苷 固相萃取 超高效液相-串联质谱 

分 类 号：TS255.7[轻工技术与工程—农产品加工及贮藏工程]