固相萃取/高效液相色谱法测定化妆品中5种抗组胺药物残留

Determination of Five Antihistamine Residues in Cosmetics by SPE/HPLC

建立了固相萃取/高效液相色谱(SPE/HPLC)测定化妆品中5种抗组胺药物(多西拉敏、曲吡那敏、溴苯那敏、苯海拉明、氯苯沙明)残留的分析方法。试样经三氯乙酸溶液超声提取,PCX柱净化后,以甲醇-磷酸盐缓冲溶液为流动相,经C18柱分离后进行HPLC检测。5种抗组胺药物在5.0～100 mg/L范围内均呈良好的线性关系,线性系数均大于0.999。在5.0、10.0、25.0 mg/kg 3个加标水平下的平均回收率为92%～108%,相对标准偏差(RSD,n=6)为2.1%～4.2%,检出限为0.5～1.0 mg/L。该方法灵敏度高、重现性好、定量准确。

A solid phase extraction coupled with high performance liquid chromatography（SPE/HPLC） was developed for the determination of five antihistamines,e.g.doxylamine,tripelennamine,brompheniramine,diphenhydramine,chlorphenoxamine,in cosmetics.The samples were extracted with trichloroacetic acid solution under ultrasonication,and cleaned up with PCX solid phase extraction.The separation of five antihistamines was carried out on a C18 column using methanol-phosphate buffer as mobile phase.The calibration curves of five drugs were linear in the range of 5.0-100 mg/L,with correlation coefficients more than 0.999.The mean recoveries at spiked levels of 5.0,10.0,25.0 mg/kg were in the range of 92%-108% with RSDs（n=6）of 2.1%-4.2%.The limits of detection were in the range of 0.5-1.0 mg/L.The method was sensitive,reproducible and accurate.