UPLC-MS/MS法检测祛痘类化妆品中7种抗生素

Determination of seven antibiotics in anti-acne cosmetics by UPLC-MS/MS

采用超高效液相色谱-三重四级杆质谱联用技术(UPLC-MS/MS)建立了祛痘类化妆品中7种抗生素(甲硝唑、盐酸美满霉素、二水土霉素、盐酸四环素、盐酸金霉素、盐酸多西环素、氯霉素)的检测方法。待测样品经超声提取、过滤稀释后,以0.1%甲酸水溶液-乙腈为流动相,BEH-C_(18)色谱柱上梯度分离,经一级、二级质谱扫描及多重反应监测(MRM)进行定性、定量分析。所建方法中,各待测组分保留时间均在2min内,检出限为0.1～1.0ng/mL,平均加样回收率为85.8%～98.5%,精密度为0.9%～3.8%。用于200批祛痘类化妆品的检测,其中9批样品检出甲硝唑和(或)氯霉素。

The UPLC-MS/MS method for determination of seven antibiotics including oxytetracycline dihydrate, tetracycline hydrochloride, minocycline hydrochloride, chlorotetracycline hydrochloride, doxycycline hydrochloride, chloramphenicol and metronidazole in anti-acne cosmetics was established. Cosmetic sample was extracted by methanol-water containing 0.1 mol/L formic acid. The extracted sample was analyzed using MS scan, Daughter scan and MRM model. These seven analytes can be separated and detected in 2 min. The detection limits are 0.1～1.0 ng/mL, and the recovery rates are 85.8%～98.5% with RSD of 0.9%～3.8%. The method has been applied to determine the antibiotics in 200 real samples from market, in which metronidazole and（or） chloramphenicol have been detected in 9 batches of samples.