高效液相色谱-高分辨率四级杆-飞行时间质谱法测定祛痘类化妆品中20种非法添加抗感染类药物
Determination of 20 Illegally Added Anti-infective Drugs in Acne Cosmetics by HPLC-Q-TOP-MS
郑篮君 1舒展 1王琤帅 1凌明 1滕云龙1
作者信息
- 1. 金华市食品药品检验检测研究院,浙江 金华 321000
- 折叠
摘要
目的:建立了采用高效液相色谱-高分辨率四级杆-飞行时间质谱(HPLC-Q-TOP-MS)法,检测祛痘类化妆品中20 种非法添加抗感染类药物的方法.方法:采用Agilent EC-C18 色谱柱(3.0×150 mm,2.7 μm);流动相为乙腈-0.1%冰醋酸溶液,梯度洗脱;流速为 0.3 mL/min;柱温为35℃;电喷雾电离源,正离子模式,根据MassHunter软件提取的保留时间、母离子、碎片离子精确质量等数据,在PCDL软件中构建了非法添加抗感染类药物的筛查数据库.结果:氯霉素和螺内酯在质量浓度 100～5000 ng/mL范围内,其余 18 种抗感染药物在质量浓度50～5000 ng/mL范围内线性关系良好(r＞0.99),检出限为 0.01～0.20 μg/g,定量限为0.05～0.80 μg/g,回收率为 83.7%～108.8%,相对标准偏差(RSD)为 1.2%～8.1%.结论:本法操作简单、准确可靠,适用于祛痘类化妆品中 20种抗感染药物的快速筛查,为祛痘类化妆品的安全监管提供了强有力的技术支撑.
Abstract
Objective:To establish a method for detecting 20 illegal anti-infective drugs in acne cosmetics by HPLC-Q-TOP-MS.Methods:An Agilent EC-C18 column(3.0×150 mm,2.7 μm)was adopted at the flow rate of 0.3 mL/min with the mobile phase was acetonitrile-0.1％glacial acetic acid solution,and the gradient eluted;The column temperature is 35℃;Positive ion mode electrospray ionization,based on the retention time,precursor ion,fragment ion accurate mass and other data extracted by MassHunter,a screening database for illegally added anti-infective drugs was constructed in PCDL.Results:Chloramphenicol and spironolactone showed a good linear relationship(r>0.99)in the range of mass concentration of 100～5000 ng/mL,while the remaining 18 anti-infective drugs showed a good linear relationship in the range of mass concentration of 50～5000 ng/mL.The detection limit was 0.01～0.20 μg/g,the quantification limit was 0.05～0.80 μg/g,the recovery rate was 83.7％～108.8％,and the relative standard deviation(RSD)was 1.2％～8.1％.Conclusion:This method is simple,accurate and reliable,and is suitable for the rapid screening of 20 anti-infective drugs in acne cosmetics,which provides strong technical support for the safety supervision of acne cosmetics.
关键词
高效液相色谱-四级杆-飞行时间质谱/非法添加/抗感染类药物/祛痘/化妆品Key words
hplc-q-top-ms/illegal additions/anti-infective drugs/acne/cosmetics引用本文复制引用
出版年
2024
NETL
NSTL
万方数据