固相萃取-液相色谱-串联质谱法测定植物油脂中香兰素  

Determination of vanillin in vegetable oil by solid phase extraction-liquid chromatography-tandem mass spectrometry

作　　者：徐彦辉 XU Yanhui(Anhui Public Inspection and Research Institute Co.,Ltd.,Hefei 230051,China)

机构地区：[1]安徽省公众检验研究院有限公司,合肥230051

出　　处：《化学分析计量》2022年第8期22-25,共4页Chemical Analysis And Meterage

摘　　要：建立了测定植物油脂中香兰素含量的固相萃取-液相色谱串联质谱法。样品经阴离子固相萃取柱净化后,利用Eclipse Plus C_(18)RRHD色谱柱(50 mm×3.0 mm,1.8μm)分离,以0.1%甲酸水溶液和甲醇为流动相梯度洗脱,流量为0.3 mL/min,柱温为35℃,液相色谱串联质谱仪在多反应监测模式下(MRM)测定,外标法定量。结果表明,香兰素的质量浓度在1~50μg/L范围内与色谱峰面积具有良好的线性关系,相关系数为0.9996,检出限为1.0μg/kg。测定结果的相对标准偏差为7.1%~8.6%(n=6),在10、50μg/kg添加水平下,空白样品加标平均回收率为102.5%和98.4%。该方法前处理过程简便快捷,准确度高,可满足实验室大批量样品快速分析的需求。A new method for the analysis of vanillin in vegetable oil by solid phase extraction-liquid chromatography-tandem mass spectrometry(LC-MS/MS)was developed.The samples were cleaned up by solid phase extraction,and separated by eclipse plus Eclipse Plus C_(18)RRHD column(50 mm×3.0 mm,1.8μm),gradient eluted with 0.1%formic acid aqueous solution and methanol as mobile phase,flow rate was 0.3 mL/min,column temperature was 35℃and then determinedby LC-MS/MS with multiple reaction monitoring and external standard method for quantification.The calibration curves were linear in the range of 1-50μg/L for vanillin,and the correlation coefficient was 0.9996.The detection limit was 1.0μg/kg.The relative standard deviation of the determination results was 7.1%-8.6%(n=6),the average recoveries of blank samples standard addtion were 102.5%and 98.4%at the level of 10 and 50μg/kg.The this method is simple of pretreatment process,fast and accurate,which can meet the needs of rapid analysis of large quantities of laboratory samples.

关 键 词：植物油脂 香兰素 液相色谱串联质谱法 

分 类 号：O657.7[理学—分析化学]