液相色谱串联质谱法同时测定化妆品中溴甲酚绿与溴百里酚蓝-海南医学.PDF

doi:10.3969/j.issn.1003-6350.2016.13.030 ·论 著· 液相色谱串联质谱法同时测定化妆品中溴甲酚绿与溴百里酚蓝 符策奕，梁颖，许文佳，陈朝曼 (海南省药品检验所化妆品室，海南 海口 570216) 【摘要】 目的 建立液相色谱串联质谱同时测定化妆品中溴甲酚绿与溴百里酚蓝的定性、定量方法。方法 样 品经甲醇超声提取，HLB 固相萃取柱分离，再通过C18 色谱柱(Kinetex C18 2.6 μm 100A 100×2.10 mm)分离，采用电喷 雾离子源及多反应监测模式(MRM)对目标化合物进行测定。结果 溴甲酚绿与溴百里酚蓝的方法检出限分别是 0.82 mg/kg、0.84 mg/kg。溴甲酚绿与溴百里酚蓝的线性范围均为0.02~4 μg/mL ，相关系数均大于0.999 5 (rBG = 1.000 0，rBB =0.999 9) ，在不同剂型的化妆品中平均回收率在98.0%~109%范围内。结论 该方法具有前处理简 单，结果准确等特点，适用于化妆品中溴甲酚绿与溴百里酚蓝的测定。 【关键词】 液相色谱串联质谱；化妆品；溴甲酚绿；溴百里酚蓝 【中图分类号】R446 【文献标识码】A 【文章编号】 1003—6350（2016 ）13—2150—04 Simultaneousdeterminationofbromocresolgreenandbromothymolblueincosmeticsbyhighperformance liquid chromatography tandem mass spectrometry. FU Ce-yi, LIANG Ying, XU Wen-jia, CHEN Chao-man. LaboratoryofCosmetics,HainanProvincialInstituteforDrugControl,Haikou570216,Hainan,CHINA 【Abstract】 Objective To develop the high performance liquid chromatography-tandem mass spectrometric method for the simultaneous determination of bromocresol green (BCG) and bromothymol blue (BTB) in cosmetics. Methods The cosmetic sample was extracted with methanol under ultrasonication, and separated by HLB solid phase extraction. The extracted complexes were separated on a C18 column (Kinetex C18, 2.6 μm, 100 A, 100×2.10 mm), and identified under electrospray ionization and multiple reactions monitoring (MRM) mode. Results The LODs of BCG and BTB are respectively 0.82 mg/kg and 0.84 mg/kg. Calibration curves were linear in the range of 0.02~4 μg/mL for BCG and BTB, with the correlation coefficients greater than 0.999 5 (rBG=1.000 0, rBB=0.999 9). The average recover- ies of BCG and BTB in different dosage forms of cosmetics ranged from 98.0%