高效液相色谱-质谱联用法同时测定染发膏中32种氧化型染料  

Determination of Thirty-Two Kinds of Oxidative Dyes in Hair Dyes by HPLC-MS/MS

作　　者：韩晶[1] 毛北萍[1] 简龙海[1] 袁晓倩 许勇[1] 郑荣[1] 陈静[1] HAN Jing;MAO Beiping;JIAN Longhai;YUAN Xiaoqian;XU Yong;ZHENG Rong;CHEN Jing(NMPA Key Laboratory for Monitoring and Evaluation of Cosmetics/Shanghai Institute of Food and Drug Control,Shanghai 201203,China)

机构地区：[1]国家药品监督管理局化妆品监测评价重点实验室/上海市食品药品检验所

出　　处：《香料香精化妆品》2020年第1期63-70,共8页Flavour Fragrance Cosmetics

摘　　要：建立了同时测定染发膏中共32种氧化型染料的高效液相色谱-质谱联用法。染发膏样品经溶剂提取,提取液经高速离心处理,上清液过净化小柱,后取续滤液经溶剂稀释,采用十八烷基硅烷键合硅胶反相色谱柱(2.1 mm×100 mm×2.7μm),以5 mmol/L乙酸铵水溶液-5 mmol/L乙酸铵乙腈溶液梯度洗脱,然后采用三重四级杆质谱测定。方法的相对标准偏差为1.0%~8.5%;回收率为71.9%~109.2%。各种氧化型染料在0.02~2.5μg/mL的质量浓度范围内均呈良好线性关系,相关系数均大于0.99。32种氧化型染料的方法检出限为20μg/g。该方法具有分离效率高、分析时间短、分析成分多等特点,已成功用于实际样品的检测。An High liquid chromatography tandem mass spectrometric(HPLC-MS/MS)method had been developed for the simultaneous determination of 32 oxidative dyes in hair dyes.Hair Dyes samples were prepared by solvent extraction,the extraction solution was obtained by high-speed centrifugation,the supernatant was filtered by purification cartridge,and the continued filtrate was diluted and then analyzed.The separation was carried out on an Agilent ODS column(2.1 mm×100 mm×2.7μm)in a gradient elution mode,with 5 mmol/L ammonium acetate aqueous solution as mobile A and 5 mmol/L ammonium acetate acetonitrile solution as the mobile phase B.An High liquid chromatography tandem mass spectrometric method was used as the determination method.The results showed that the relative standard deviations(RSD)were 1.0%to 8.5%;recoveries were 71.9%to 109.2%;The linear range of various oxidative dyes showed good linearity within the concentration ranges of 0.02 to 2.5μg/mL,correlation coefficients were greater than 0.996;detection limits were 20μg/g.This method has the advantages of high efficiency,short analytical time and realized analysis of multiple components simultaneously.It has been successfully used for analyzing the commercial products.

关 键 词：高效液相色谱-质谱联用法 氧化型染料 染发膏 

分 类 号：O657.63[理学—分析化学] TQ658.34[理学—化学]