固相萃取/超高效液相色谱-串联质谱法测定儿童化妆品中新康唑等4种抗生素  

Simultaneous Determination of 4 Antibiotics in Children’s Cosmetics by Ultra-performance Liquid Chromatography-Tandem Mass Spectrometry with Solid Phase Extraction

作　　者：汪毅 聂明霞 贾芳 梁文耀 李鑫宇 文嘉林 夏泽敏 谭建华 WANG Yi;NIE Ming-xia;JIA Fang;LIANG Wen-yao;LI Xin-yu;WEN Jia-lin;XIA Ze-min;TAN Jian-hua(National Quality Inspection and Testing Center for Cosmetics(Guangzhou),Guangzhou Quality Supervision and Testing Institute,Guangzhou 511447,China)

机构地区：[1]广州质量监督检测研究院,国家化妆品质量检验检测中心,广东广州511447

出　　处：《分析测试学报》2022年第12期1746-1750,共5页Journal of Instrumental Analysis

摘　　要：建立了测定儿童化妆品中新康唑等4种抗生素的超高效液相色谱-串联质谱法(UPLC-MS/MS)。样品经70%乙腈水溶液超声提取后,使用SCX固相萃取小柱净化,以0.1%甲酸水和乙腈作为流动相,经Waters AC⁃QUITY BEH C_(18)(2.1 mm×100 mm,2.5μm)色谱柱分离,使用多反应监测模式(MRM)进行测定。结果表明,4种抗生素线性关系良好,相关系数(r)均为0.999,方法检出限(LOD)和定量下限(LOQ)分别为0.005~0.250μg/g和0.010~0.500μg/g。4种抗生素在3种基质和3个加标水平的平均回收率为89.3%~113%,相对标准偏差(RSD)为0.90%~7.2%。该方法高效、准确、特异性好,满足新康唑等4种抗生素在儿童化妆品中的测定需求。An ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was established for the determination of 4 antibiotics in children’s cosmetics.The cosmetic samples were extracted with 70%acetonitrile-water solution,and then purified with a SCX column.The target analytes were separated on a Waters ACQUITY BEH C_(18)(2.1 mm×100 mm,2.5μm)column using 0.1%formic acid solution and acetonitrile as mobile phases.The analysis was per⁃formed under multiple reaction monitoring(MRM)mode.Results showed that there were good linear relationships for 4 antibiotics in the respective concentration ranges with their correlation coefficients(r)of 0.999.The limits of detection(LODs)and limits of quantitation(LOQs)of the method were in the range of 0.005-0.250μg/g and 0.010-0.500μg/g,respectively.Average recoveries for the 4 antibiotics in 3 kinds of samples at 3 spiked levels ranged from 89.3%to 113%,with relative stan⁃dard deviations(RSDs,n=6)of 0.90%-7.2%.The method is effective,accurate and specific,and it could be used for the determination of 4 antibiotics in children’s cosmetics.

关 键 词：抗生素 儿童化妆品 超高效液相色谱-串联质谱法(UPLC-MS/MS) 净化 

分 类 号：O657.7[理学—分析化学] TQ658[理学—化学]