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.
作者
陆土柳
李静
陈张好
周智明
Lu Tuliu;Li Jing;Chen Zhanghao;Zhou Zhiming(Guangdong Institute for Drug Control,Guangzhou 510525,China)
出处
《广东化工》
CAS
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)。