液相色谱-三重四极杆复合线性离子阱质谱法测定烟用香精香料中9种有机酸的含量  

Determination of 9 Organic Acids in Tobacco Flavors by Liquid Chromatography-Triple Quadrupole Composite Linear Ion Trap Mass Spectrometry

作　　者：陈晓水[1] 苏燕[1] 汤晓东[1] 蒋佳磊[1] 张丽娜[1] 朱书秀[1] 许式强 刘崇盛 CHEN Xiaoshui;SU Yan;TANG Xiaodong;JIANG Jialei;ZHANG Lina;ZHU Shuxiu;XU Shiqiang;LIU Chongsheng(China Tobacco Zhejiang Industrial Co.,Ltd.,Hangzhou 310024,China)

机构地区：[1]浙江中烟工业有限责任公司,杭州310024

出　　处：《理化检验（化学分册）》2024年第10期1033-1039,共7页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：浙江中烟工业有限责任公司科技项目(ZJZY2022C003、ZJZY2021A002)。

摘　　要：采用液相色谱-三重四极杆复合线性离子阱质谱法定性定量检测烟用香精香料中苹果酸、柠檬酸、乳酸、丙二酸、琥珀酸、马来酸、酒石酸、己二酸、乙酰丙酸等9种有机酸。取0.1 g烟用香精香料样品,加入20 mL水,超声提取10 min。取上清液1 mL,过0.22μm水相滤膜后用水稀释10倍,按照优化的仪器工作条件测定。在Synergi Hydro-RP色谱柱上用不同体积比的0.1%(体积分数,下同)甲酸溶液和含0.1%甲酸的甲醇溶液的混合液梯度洗脱分离各有机酸后,用电喷雾离子源负离子模式电离,多反应监测-信息依赖采集-增强子离子(MRM-IDA-EPI)模式扫描,MRM模式定量,保留时间结合EPI标准品二级质谱库定性。结果表明:9种有机酸的质量浓度均在一定范围内和定量子离子峰面积呈线性关系,检出限(3s/k)为0.003~0.018 mg·L^(-1);对实际样品进行加标回收试验,回收率为73.3%~112%,日内(n=6)、日间(n=5)精密度试验所得测定值的相对标准偏差分别不大于10%和不大于15%;方法用于142种烟用香精香料样品的分析,检出率较高的4种有机酸为乳酸、苹果酸、琥珀酸和柠檬酸。The 9 organic acids,including malic acid,citric acid,lactic acid,malonic acid,succinic acid,maleic acid,tartaric acid,adipic acid and levulinic acid,in tobacco flavor samples were determined qualitatively and quantitatively by liquid chromatography-triple quadrupole composite linear ion trap mass spectrometry.The 0.1 g of tobacco flavor sample was taken,and 20 mL of water was added.After extracting by ultrasound for 10 min,1 mL of the supernatant was taken,and passed through a 0.22μm aqueous phase membrane.The solution obtained was diluted 10 times with water for determination according to the optimized instrument operating conditions.Organic acids were separated by gradient elution with mixed solutions of 0.1%(volume fraction,the same below)formic acid solution and methanol solution containing 0.1%formic acid at different volume ratios on the Synergi Hydro-RP chromatographic column,ionized by negative ion mode of electrospray ion source,scanned by the multiple reaction monitoring-information dependent acquisition-enhanced product ion(MRM-IDA-EPI)mode,quantified by MRM mode,and qualitatively analyzed by combining EPI standard secondary mass spectrometry library with retention time.It was shown that linear relationships between values of the mass concentrations of 9 organic acids and peak areas of quantitative daughter ions were kept in definite ranges,with detection limits(3s/k)in the range of 0.003-0.018 mg·L^(−1).Test for recovery was conducted on actual samples by the standard addition method,with recoveries ranging from 73.3%to 112%.RSDs of the determined values obtained from intra-day(n=6)and inter-day(n=5)precision tests were not exceed 10%or 15%,respectively.The proposed method was applied to the analysis of 142 tobacco flavor samples,and 4 organic acids with the higher detection rates were lactic acid,malic acid,succinic acid and citric acid.

关 键 词：烟用香精香料 有机酸 液相色谱-三重四极杆复合线性离子阱质谱法 多反应监测-信息依赖采集-增强子离子(MRM-IDA-EPI)扫描 

分 类 号：O657.63[理学—分析化学]