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 in Cosmetics by HPLC-MS/MS
陆土柳 1李静 1陈张好 1周智明1
作者信息
- 1. 广东省药品检验所,广东 广州 510525
- 折叠
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C18 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(r2)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.
Abstract
To combat the illegal addition of antibacterial drug synergists in cosmetics,an HPLC-MS/MS detection method for five antibacterial synergists in cosmetics 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 a C18 chromatographic column,using an electrospray ionization source.Both positive and negative ion multiple reaction monitoring(MRM)modes is employed for chromatographic analysis.The results show that the five antibacterial synergists exhibit a good linear relationship within the mass concentration range of 0.1 mg/L to 2 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 found to contain trimethoprim at a mass fraction of 7.9%.This method is characterized by simple pretreatment,high analytical efficiency,and accurate results,providing a technical 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Key words
HPLC-MS/MS/antibacterial drug synergists/acne cosmetics/multiple reaction monitoring mode/trimethoprim引用本文复制引用
出版年
2024
NETL
NSTL
万方数据