同位素稀释-超高效液相色谱-串联质谱法测定化妆品中香兰素和乙基香兰素  

Determination of vanillin and ethyl-vanillin in cosmetics by isotope dilutionultra performance liquid chromatography-tandem mass spectrometry

作　　者：黄键 王金娟 周元元 张敏 王红卫 王晓颖 孙雪婷 HUANG Jian;WANG Jinjuan;ZHOU Yuanyuan;ZHANG Min;WANG Hongwei;WANG Xiaoying;SUN Xueting(Nantong Customs Comprehensive Technology Center,Nantong 226004,China)

机构地区：[1]南通海关综合技术中心,江苏南通226004

出　　处：《化学分析计量》2023年第6期34-39,共6页Chemical Analysis And Meterage

基　　金：南通市科技计划项目(JC2020112)。

摘　　要：建立同位素稀释-超高效液相色谱-串联质谱法同时测定化妆品中两种香兰素类香料的方法。取1g样品,加入50μL质量浓度均为1mg/L的香兰素-D3、乙基香兰素-D5混合同位素内标溶液,以甲醇为提取溶剂,溶解后定容至10mL,在室温下超声提取15min,离心分离后,取1mL上清液用氮气吹干,再用1mL0.1%甲酸水溶液-甲醇(体积比为80∶20)定容,过滤后上机分析。经RRHDEclipsePlusC18色谱柱分离后,使用ESI源对目标物进行电离,在多反应监测模式下绘制色谱图,内标法定量。在5~100μg/L范围内,香兰素、乙基香兰素与内标的质量浓度比与对应色谱峰面积的比线性关系良好,相关系数均大于0.999,方法检出限均为5μg/kg。空白样品加标回收率分别为87.8%~96.1%、80.1%~83.8%,测定结果的相对标准偏差分别为2.5%~3.8%、1.7%~4.6%(n=6)。该方法操作简便,可满足同时测定化妆品中两种香兰素类香料的要求。A method for simultaneous determination of vanillin and ethyl-vanillin in cosmetics by isotope dilution-ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was established.50μL isotope internal standard mixed solution contained 1 mg/L vanillin-D3 and 1 mg/L ethyl-vanillin-D5 was added to the sample,then the sample was dissolved,made up to 10 mL by methanol,and extracted by ultrasonic in room temperature for 15 min.After centrifugal separation,1 mL supernate was dried by nitrogen and diluted with 1 mL solution consisted of 0.1%formic acid and methanol(volume ratio was 80∶20).Then the solution was filtrated by 0.22 mm filter membrane and injected directly.The analytes were separated by RRHD Eclipse Plus C18 column,ionized by ESI source,detected by MRM mode,and finally quantified with internal standard method.In the range of 5-100μg/L,the mass concentration ratio of vanillin,ethyl vanillin and internal standards had a good linear relationship with the ratio of the corresponding chromatographic peak area,the correlation coefficients were all more than 0.999,and the determination limits were 5μg/kg.The recoveries of blank samples were 87.8%-96.1%、80.1%-83.8%,respectively.The relative standard deviations of the determination results were 2.5%-3.8%、1.7%-4.6%(n=6),respectively.This method is simple,which can provide a useful tool for the determination of vanillin and ethyl-vanillin in cosmetics.

关 键 词：同位素稀释 超高效液相色谱-串联质谱法 香兰素 乙基香兰素 化妆品 

分 类 号：O657.7[理学—分析化学]