高效液相色谱串联质谱法测定化妆品中15种喹诺酮类抗生素  

Determination of 15 quinolone antibiotics in cosmetics by liquid chromatography tandem mass spectrometry

作　　者：卢剑[1] 寻知庆 汪晨霞 郭新东 杨洋[1] 武中平[1] LU Jian;XUN Zhi-qing;WANG Chen-xia;GUO Xin-dong;YANG Yang;WU Zhong-ping(Jiangsu Product Quality Inspection and Testing Institute, Nanjing, Jiangsu 210007, China;Guangzhou Quality Supervision and Testing Institute, Guangzhou, Guangdong 511447, China)

机构地区：[1]江苏省产品质量监督检验研究院,江苏南京210007 [2]广州质量监督检测研究院,广东广州511447

出　　处：《日用化学工业》2019年第6期403-409,共7页China Surfactant Detergent & Cosmetics

基　　金：质检公益性行业科研专项项目资助(201410230)

摘　　要：利用液液萃取和高效液相色谱串联质谱仪(HPLC-MS/MS),建立了化妆品中15种喹诺酮类抗生素的HPLC-MS/MS分析方法。样品使用0.1%甲酸乙腈溶液提取,正己烷除脂,经Thermo Hypersil GOLD C18(2.1 mm×100 mm,1.9 μm)色谱柱分离后,三重四级杆质谱多反应监测模式(MRM)检测,以保留时间和相对离子丰度定性,外标法定量。结果表明,15种喹诺酮类抗生素在质量浓度5.0~200 μg/L范围内呈现良好的线性关系,相关系数均大于0.995 0;方法检出限和定量限分别为0.15和0.50 mg/kg。样品平均加标回收率在80.1%~104.9%之间,精密度(RSD,n=6)为1.0%~7.4%。该方法检出限、回收率和精密度满足化妆品中喹诺酮类抗生素的测定。A high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS) method was established for the determination of 15 quinolone antibiotics in cosmetics. The samples were extracted with 0.1% formic acid acetonitrile solution, degreased with n-hexane, separated by Thermo Hypersil GOLD C18(2.1 mm×100 mm, 1.9 μm) column, then detected by triple quadrupole mass spectrometry multi-reaction monitoring mode(MRM) to determine retention time and relative ion abundance, and quantified by external standard method. The results show that all of the 15 quinolone antibiotics show good linearity in the range of 5.0-200 μg/L with the correlation coefficients greater than 0.995 0. The limit of detection and quantification of the method are 0.15 and 0.50 mg/kg, respectively. The average recoveries of the spiked samples were ranged from 80.1% to 104.9% and the relative standard deviations(RSD, n=6) were in the range of 1.0%-7.4%. The method is accurate and reliable, which meets the requirements of the determination of quinolone antibiotics in cosmetics.

关 键 词：高效液相色谱串联质谱 化妆品 抗生素 喹诺酮 

分 类 号：TQ658[化学工程—精细化工]