超高效液相色谱-差分离子淌度质谱法测定化妆品中10种卡因类禁用组分  

Determination of 10 Kinds of Caine-Type Prohibited Ingredients in Cosmetics by Ultra-Performance Liquid Chromatography-Differential Mobility Spectrometry-Mass Spectrometry

作　　者：连显会 王春 孟宪双[1] 白桦[1] 孙小杰 薛宏宇 马强[1] LIAN Xian-Hui;WANG Chun;MENG Xian-Shuang;BAI Hua;SUN Xiao-Jie;XUE Hong-Yu;MA Qiang(Chinese Academy of Inspection and Quarantine, Beijing 100176, China;School of Life Science and Medicine, Dalian University of Technology, Panjin 124221, China;College of Resources and Environmental Sciences, Nanjing Agricultural University, Nanjing 210095, China;SCIEX Asia Pacific Application Support Center, Beijing 100015, China)

机构地区：[1]中国检验检疫科学研究院,北京100176 [2]大连理工大学生命与医药学院,盘锦124221 [3]南京农业大学资源与环境科学学院,南京210095 [4]SCIEX亚太技术支持中心,北京100015

出　　处：《分析化学》2019年第5期756-764,共9页Chinese Journal of Analytical Chemistry

基　　金：国家重点研发计划项目(No.2016YFF0203701);国家标准化管理委员会计划项目(No.20173894-T-607)资助~~

摘　　要：建立了化妆品中10种卡因类禁用组分的超高效液相色谱-差分离子淌度质谱测定方法。以正十二醇为萃取剂、四氢呋喃为分散剂在水中自组装形成超分子溶剂,并结合涡旋辅助对化妆品试样进行分散液液微萃取。考察了超分子溶剂的组成、用量及涡旋时间等参数对萃取效率的影响,以及差分离子淌度质谱对同分异构体的分离效果。结果表明,试样在4 mL正十二醇-四氢呋喃超分子溶剂中涡旋振荡3 min即可完成高效萃取,且可有效去除基质干扰,降低基质效应。差分离子淌度质谱在优化的载气、分离电压、补偿电压等条件下可将色谱难以分离的同分异构体(苯佐卡因和三卡因)实现淌度分离,解决了两种同分异构体由于色谱无法分离而不能准确定性和定量分析的问题。10种卡因类组分在各自浓度范围内线性关系良好,相关系数均大于0.99,方法检出限为0.2～8.0μg/kg,方法定量限为0.4～20.0μg/kg。在低、中、高3个添加水平下的平均回收率为70.7%～94.7%,相对标准偏差为1.2%～12.7%(n=6)。本方法步骤简便、快速高效,适用于化妆品中10种卡因类禁用组分的同时分析测定。An analytical method for determination of 10 kinds of caine-type prohibited ingredients in cosmetics was developed using supramolecular solvent-based dispersive liquid-liquid microextraction followed by ultra-performance liquid chromatography coupled with differential mobility spectrometry-mass spectrometry. The supramolecular solvent was prepared with dodecanol as extraction solvent and tetrahydrofuran as dispersing agent for dispersive liquid-liquid microextraction of cosmetic samples under vortexing. The effects of the composition and amount of supramolecular solvent and vortex time on the extraction efficiency and the separation of isomers by differential mobility spectrometry were systemitically investigated. Results showed that the sample could be effectively extracted by 4 mL of supramolecular solvent consisting of dodecanol and tetrahydrofuran after vortexing for 3 min. Under the optimized conditions including carrier gas, separation voltage and compensation voltage, the isomers of benzocaine and tricaine could be well separated by differential mobility spectrometry for qualitative confirmation and quantitative determination, which could hardly be chromatographically separated. The 10 kinds of caine-type compounds exhibited good linearity in their respective concentration ranges, with correlation coefficients of better than 0.99. The limits of detection and quantitation were 0.2-8.0 μg/kg and 0.4-20.0 μg/kg, respectively. The average recoveries at low, medium and high spiked levels ranged from 70.7% to 94.7% with relative standard deviations of 1.2% to 12.7%( n =6). The method is simple, rapid, efficient, and is suitable for the simultaneous determination of the 10 kinds of caine-type prohibited ingredients in cosmetics.

关 键 词：超分子溶剂 分散液液微萃取 化妆品 差分离子淌度质谱 

分 类 号：O657.63[理学—分析化学]