基于QuEChERS提取的液相色谱-串联质谱法测定化妆品中11种抗真菌药物残留  

QuEChERS-based liquid chromatography coupled with triple quadrupole mass spectrometry for the determination of eleven antifungal drugs in cosmetics

作　　者：邵明媛[1] 王浩[1] 史海良[1] 杨红梅[1] 

机构地区：[1]国家食品质量安全监督检验中心,北京100094

出　　处：《分析试验室》2016年第4期430-434,共5页Chinese Journal of Analysis Laboratory

基　　金：国家质检总局公益项目专项(201410230-03)资助

摘　　要：建立了化妆品中酮康唑、伏立康唑、克霉唑、联苯苄唑、伊曲康唑、益康唑、咪康唑、特康唑、氟康唑、奥西康唑和芬替康唑等11种唑类抗真菌药物的液相色谱-串联质谱测定方法。样品经过改良的Qu ECh ERS方法提取净化、液相色谱-串联质谱仪进行测定、基质外标法定量。在40~400μg/kg和800~8000μg/kg的线性范围内,线性相关系数（R2）〉0.99,3个不同浓度添加水平下的加标回收率为75.1%~107.4%,相对标准偏差（RSD）为1.0%~11%（n=6）。化妆品中咪康唑、伏立康唑、克霉唑、联苯苄唑、芬替康唑、氟康唑、益康唑的检出限为10.0μg/kg,定量限为40.0μg/kg;酮康唑、特康唑、奥西康唑、伊曲康唑的检出限为200.0μg/kg,定量限为800.0μg/kg。采用建立的方法对市面上销售的130余种化妆品中11种抗真菌药物进行了筛查,达到预期效果。方法可适用于化妆品中多种抗真菌药物的快速分析。A rapid method was established and applied to the extraction of eleven antifungal drugs in cosmetics prior to the determination by liquid chromatography coupled to triple quadrupole mass spectrometry（ HPLC-MS /MS）. The antifungal drugs were extracted from the cosmetic samples using the modified Qu ECh ERS method without any further clean-up step. The separation of the analytes was carried out on an Agilent XDB C8 column（ 150 mm× 2. 1 mm,1. 8 μm） using the mobile phases of methanol and 1%（ volume percentage） formic acid aqueous solution with gradient elution at a flow rate of 0. 3 m L / min. Finally the samples were determined by HPLC-MS / MS.Matrix-matched calibration was used for the quantification. The proposed method showed good linearity with the correlation coefficients all above 0. 99. The recoveries of eleven antifungal drugs obtained by analyzing the three spiked levels were in the range of 75. 1% ~ 107. 4% with the RSDs ranging from 1. 0 to 11%. Seven sensitive antifungal drugs＇ s limits of detection were 10 μg / kg and the limit of quantitation were 40 μg / kg. The limits of detection were 200 μg / kg and the limit of quantitation were 800 μg / kg for the other four antifungal drugs. The developed method was successfully applied for antifungal drugs analysis in more than 130 samples. The present method was accurate and sensitive for the determination of a variety of antifungal drugs residues in cosmetics.

关 键 词：QUECHERS 液相色谱-串联质谱 抗菌素 化妆品 

分 类 号：R917[医药卫生—药物分析学]