高效液相色谱-串联质谱法测定化妆品中17种头孢类抗生素

Determination of 17 cephalosporins residues in cosmetics by HPLC-MS-MS

建立了高效液相色谱-串联质谱(HPLC-MS/MS)测定化妆品中的17种头孢类抗生素的方法。化妆品中的头孢类药物使用EDTA-Mcllvaine缓冲液提取,经超声和离心后,上清液经PRIME HLB固相萃取柱净化。采用Waters ACQUITY UPLC BEH C18 (2.1 mm×100 mm,1.7μm)色谱柱分离,流动相为甲醇-0.1%甲酸水溶液,梯度洗脱,电喷雾离子源正离子模式,多反应监测模式(MRM)进行检测。结果表明,17种头孢类药物在此分析方法下分离效果良好,在相应的范围内线性关系良好,相关系数均大于0.99,各加标水平的平均回收率为75.27%~110.32%,相对标准偏差小于10.00%。该方法前处理方便简单,定量准确,适用于化妆品基质中头孢类抗生素的测定。

There is a huge space in the market of cosmetics,and the quality problem of antibiotics abusage in cosmetics often exists.Cephalosporins as a kind of antibiotic have also been found in cosmetics regulation in recent years.Currently there is no literature on the determination method of cephalosporins in cosmetics.In order to assess the cephalosporins residues in cosmetics,a method was established for the determination of 17 cephalosporins residues in cosmetics by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The cosmetics with liquid water-based,oil-based and cream were investigated.The conditions of extractant solvent,solid phase extraction column and chromatographic conditions were optimized.The samples were ultrasonically extracted with EDTA-Mcllvaine,centrifuged,and then purified with PRIME HLB SPE columns.The target compounds were separated on a Waters ACQUITY UPLC BEH C18 column(2.1 mm×100 mm,1.7 μm) by gradient elution using methanol and 0.1% formic acid solution as mobile phases.The analysis was carried out using a positive electrospray ion source in the multiple reaction monitoring mode.Results show that under the optimized test conditions the target compounds are separated effectively.There are good linear relationships for 17 cephalosporins in the corresponding ranges,and the linear correlation coefficients are all above 0.99.The average recoveries of the lower limit of quantitation are between 75.27% and 110.32%,and the relative deviations are less than 10.00%.The method is convenient,simple,accurate,and is suitable for the determination of 17 cephalosporins in various kinds of cosmetics.