高效液相色谱-串联质谱法测定化妆品中3种甲基咪唑类化合物  

Determination of three methylimidazole compounds in cosmetics by high performance liquid chromatography-tandem mass spectrometry

作　　者：蔡翠玲 李菊 席静 侯颖烨 曾广丰 谢建军 吴舒悦 王璐 CAI Cuiling;LI Ju;XI Jing;HOU Yingye;ZENG Guangfeng;XIE Jianjun;WU Shuyue;WANG Lu(Guangzhou Customs Technical Center,National Import and Export Food Quality Safety Risk Verification and Evaluation Laboratory(Cosmetics),Guangzhou 510623,China)

机构地区：[1]广州海关技术中心,国家级进出口食品质量安全风险验证评价实验室(化妆品),广东广州510623

出　　处：《色谱》2024年第11期1052-1058,共7页Chinese Journal of Chromatography

基　　金：广州海关科研项目(2021GZCK19).

摘　　要：建立了一种同时测定化妆品中1-甲基咪唑(1-MEI)、2-甲基咪唑(2-MEI)和4-甲基咪唑(4-MEI)的高效液相色谱-串联质谱(HPLC-MS/MS)方法。样品经乙腈提取、混合型阳离子交换(MCX)固相萃取柱净化、氮吹及复溶后,使用XBridge shield RP 18色谱柱(150 mm×4.6 mm,3.5μm)进行分离;以含0.1%甲酸的20 mmol/L甲酸铵水溶液-乙腈(98∶2,v/v)作为流动相进行等度洗脱;质谱分析采用电喷雾电离(ESI)源和多反应监测(MRM)模式,外标法定量。结果表明,1-MEI在5~200μg/L范围内线性关系良好(相关系数(r^(2))≥0.9994),2-MEI和4-MEI在2~100μg/L范围内线性关系良好(r^(2)≥0.9984)。3种甲基咪唑类化合物的检出限(LOD)为10~30μg/kg,定量限(LOQ)为25~100μg/kg。在低、中、高3个加标水平下,不同空白基质中3种甲基咪唑类化合物的回收率为80.9%~107.9%,相对标准偏差(RSD,n=6)为1.2%~12.8%。将该方法应用于48个化妆品样品的检测,结果表明,有9个样品检出4-MEI,检出含量为26~1000μg/kg;2个样品检出2-MEI,检出含量分别为240μg/kg和267μg/kg;而48个样品中均未检出1-MEI。该方法简单、快速,灵敏度高,为化妆品中3种甲基咪唑类化合物的风险评估和筛查监测提供了技术支撑。Methylimidazole compounds are byproducts formed during the caramel-coloring process and are used in various cosmetics.In addition metronidazole is an antibacterial and anti-inflammatory drug commonly used in modern medicine and is used in cosmetics to treat acne in the short-term.The illegal addition of metronidazole during cosmetics production can result in residual 2-methylimidazole(2-MEI),which,along with 4-methylimidazole(4-MEI),is a class 2B carcinogen.Therefore,establishing efficient,accurate,and sensitive analytical techniques for analyzing methylimidazole compounds in cosmetics is an urgent objective.In this study,a high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method for simultaneously determining 1-methylimidazole(1-MEI),2-MEI,and 4-MEI in cosmetics was developed.Cosmetics samples were extracted via ultrasonication in acetonitrile and purified using a mixed cation-exchange(MCX)solid-phase extraction(SPE)column,with subsequent drying under a stream of nitrogen and redissolution in acetonitrile.The resulting solution was then filtered through a 0.22μm organic filter membrane for further testing.The analytes were separated using an XBridge shield RP 18 chromatographic column(150 mm×4.6 mm,3.5μm)and isocratically eluted with 20 mmol/L ammonium formate solution(containing 0.1%formic acid)-acetonitrile(98∶2,v/v).The target compounds were ionized by electrospray ionization(ESI)source,analyzed in multi-reaction monitoring(MRM)mode,and quantified using the external standard method,with the peak area of the quantitative ion and the mass concentration of the compound taken as the longitudinal and transverse coordinates,respectively.Matrix-matching working curves were also constructed.1-MEI exhibited good linear relationships in the range of 5-200μg/L,with correlation coefficients(r^(2))≥0.9994,while 2-MEI and 4-MEI showed good linearities in the range of 2-100μg/L with r^(2)≥0.9984.The three methylimidazole compounds exhibited limits of detection(LODs)and quantification(LOQs

关 键 词：高效液相色谱-串联质谱 1-甲基咪唑 2-甲基咪唑 4-甲基咪唑 化妆品 

分 类 号：O658[理学—分析化学]