摘要
该文基于超高效液相色谱-串联质谱(UPLC-MS/MS)建立了化妆品中34种β-内酰胺类抗生素的分析方法。样品经20%乙腈溶液提取,正己烷萃取除去脂溶性杂质,离心后取下层溶液,采用Agilent ZORBAX SB-Aq色谱柱(2.1 mm×100 mm,1.8μm)分离,以0.2%甲酸溶液-乙腈为流动相进行梯度洗脱,经电喷雾电离(ESI),正负离子扫描,多反应监测(MRM)模式检测,基质匹配标准曲线进行定量分析。结果显示,34种β-内酰胺类抗生素在相应的质量浓度范围内呈良好的线性关系(r>0.995),方法检出限为0.03~1.5μg·g^(-1),定量下限为0.1~5μg·g^(-1),膏霜、乳液、水剂、凝胶4种化妆品基质在低、中、高3个加标水平下的平均回收率为85.9%~111%,相对标准偏差(RSD,n=6)为0.90%~8.0%。该方法简便、快速、灵敏、准确,可用于化妆品中34种β-内酰胺类抗生素的检测,为化妆品质量控制和市场监管提供技术支持。
In this study,a method for the analysis of 34β-lactam antibiotics in cosmetics was estab⁃lished based on ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The samples were extracted with 20%acetonitrile solution,and lipophilic impurities were re⁃moved by n-hexane extraction.After centrifugation,the lower layer solution was collected and sepa⁃rated using an Agilent ZORBAX SB-Aq column(2.1 mm×100 mm,1.8μm)with a mobile phase of 0.2%formic acid solution and acetonitrile in gradient elution.Analyzed by electrospray ionization source(ESI)in both positive and negative ion modes,with multiple reaction monitoring(MRM),and matrix matching curves were used for quantitative analysis.The results showed good linearity(r>0.995)for 34β-lactam antibiotics in corresponding concentration ranges.The limits of detection(LODs)and quantitation(LOQs)were 0.03-1.5μg∙g^(-1) and 0.1-5μg∙g^(-1),respectively.The aver⁃age recoveries of four cosmetic matrices(cream,emulsion,aqueous,gel)at three different spiked levels ranged from 85.9%to 111%,with relative standard deviations(RSDs,n=6)of 0.90%-8.0%.The method is simple,rapid,sensitive and accurate and can be used for the determination of 34β-lac⁃tam antibiotics in cosmetics,which could provide technical support for the quality control and market supervision of cosmetics.
作者
程佳华
陈旭
简育莹
谢宋阳
卢端萍
陈硕
CHENG Jia-hua;CHEN Xu;JIAN Yu-ying;XIE Song-yang;LU Duan-ping;CHEN Shuo(Fujian Institute for Food and Drug Quality Control,Fuzhou 350012,China)
出处
《分析测试学报》
2026年第2期320-328,共9页
Journal of Instrumental Analysis
基金
福建省市场监督管理局科技项目(FJMS2024048)。
关键词
超高效液相色谱-串联质谱法
化妆品
β-内酰胺类抗生素
头孢类抗生素
青霉素类抗生素
非法添加
ultra performance liquid chromatography-tandem mass spectrometry
cosmetics
β-lac⁃tam antibiotics
cephalosporin antibiotics
penicillin antibiotics
illegal addition
