HPLC-MS/MS法同时测定化妆品中5种抗菌类药物增效剂  

Simultaneous Measurement of Five Antibacterial Drug Synergists inCosmetics by HPLC-MS/MS

作　　者：陆土柳 李静[1] 陈张好[1] 周智明 Lu Tuliu;Li Jing;Chen Zhanghao;Zhou Zhiming(Guangdong Institute for Drug Control,Guangzhou 510525,China)

机构地区：[1]广东省药品检验所,广东广州510525

出　　处：《广东化工》2024年第23期125-128,共4页Guangdong Chemical Industry

基　　金：广东省食品药品监督管理局科技创新项目(ZA20230015);广东省药品监督管理局化妆品风险评估重点实验室专项(2023ZDZ11)。

摘　　要：为打击化妆品中非法添加抗菌类药物增效剂的行为,建立了化妆品中5种抗菌增效剂的HPLC-MS/MS检测方法。样品(包含水剂及膏剂)经过甲醇溶解超声提取后,以甲醇-质量分数1%乙酸溶液作为流动相梯度洗脱,流速为0.3 mL/min,在C_(18)色谱柱上进行洗脱分离,采用电喷雾离子源,同时采取正和负离子多反应监测模式(MRM)进行色谱分析。结果表明,5种抗菌增效剂在质量浓度0.1 mg/L~2 mg/L范围内线性关系良好,其线性相关系数(r^(2))均大于0.99。在祛痘化妆品基质中进行加标回收试验,方法的回收率为88%~120%,方法的相对标准偏差为2.4%~9.1%,精密度良好(RSD<2%)。对99批次祛痘类化妆品进行检验,其中1批次检出甲氧苄啶,质量分数为7.9%。该方法前处理简单,分析效率高,结果准确,为化妆品中5种抗菌类药物增效剂的质量控制提供了技术参考。To combat the illegal addition of antibacterial drug synergists in cosmetics,an HPLC-MS/MS detection method for five antibacterial synergists incosmetics has been established.After the samples(including water-based and cream-based products)are dissolved and ultrasonically extracted in methanol,methanol-1%acetic acid solution by mass is used as the mobile phase for gradient elution at a flow rate of 0.3 mL/min.The elution and separation is carried out on aC_(18) chromatographic column,using an electrospray ionization source.Both positive and negative ion multiple reaction monitoring(MRM)modes is employed forchromatographic analysis.The results show that the five antibacterial synergists exhibit a good linear relationship within the mass concentration range of 0.1 mg/L to2 mg/L,with linear correlation coefficients(r2)greater than 0.99.Conduct spiked recovery tests in the matrix of acne removing cosmetics,the recovery rate was 88%~120%,the relative standard deviation of 2.4%to 9.1%,and the precision was good(RSD<2%).Among 99 batches of acne cosmetics tested,one batch was foundto contain trimethoprim at a mass fraction of 7.9%.This method is characterized by simple pretreatment,high analytical efficiency,and accurate results,providing atechnical reference for the quality control of five antibacterial drug synergists in cosmetics.

关 键 词：HPLC-MS/MS 抗菌类药物增效剂 祛痘类化妆品 多反应监测模式 甲氧苄啶 

分 类 号：TQ658[化学工程—精细化工] O657.72[理学—分析化学]