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

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。

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

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 271.2>108.0 as quantitative ion pair and m/z 271.2>160.9 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.