超高效液相色谱-串联质谱法测定化妆品中4种烯丙胺类抗真菌药物质量的含量
Determination of Four Allylamine Antifungal Drugs in Cosmetics by UPLC-MS/MS
刘轩彤 1王天歌 1赵迎春1
作者信息
- 1. 沈阳市食品药品检验所,辽宁沈阳 110000
- 折叠
摘要
采用超高效液相色谱-串联质谱法(UPLC-MS/MS)建立化妆品中烯丙胺类药物布替萘芬、萘替芬、特比萘芬、托萘酯的检测方法.以体积分数 80%乙腈水溶液为提取溶剂经涡旋和超声提取,上清液经微孔滤膜过滤后测定.用Waters Acquity UPLC® BEH-C18(100 mm×2.1 mm×1.7 μm)色谱柱,以体积分数1%甲酸水溶液-乙腈为流动相进行梯度洗脱,流速为 0.3 mL/min,采用多反应离子监测(MRM)模式进行定性定量分析.这 4 种抗真菌药物的质量浓度在 0.1～32 ng/mL时,均与响应值呈良好的线性关系,相关系数均大于 0.995,检出限为 1.737～1.815 ng/g,定量限为5.212～5.445 ng/g,在低、高浓度范围内加标回收率为96.78%～113.22%,相对标准偏差(RSD)为0.6%～4.8%.
Abstract
A method was established for the determination of allylamine drugs butenafine,naftifine,terbinafine and tolnaphthyl ester,in cosmetics by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The extract was vortexed and ultrasonically extracted with 80%(in volume)acetonitrile.The supernatant was filtered through a micro porous membrane and determined.Waters Acquity UPLC® BEH-C18(100 mm×2.1 mm×1.7 μm)chromatographic column was used for gradient elution with 1%(in volume)formic acid aqueous solution-acetonitrileas mobile phase at a flow rate of 0.3 mL/min.Qualitative and quantitative analyses were performed by multiple reaction ion monitoring(MRM)mode.When the mass concentration of four antifungal drugs in 0.1-32 ng/mL,the regression equations showed good linear relationship.The correlation coefficients were all greater than 0.995.The detection limits were 1.737-1.815 ng/g and the quantitative limits were 5.212-5.445 ng/g.In the low and high concentration ranges,the recovery rate was 96.78%-113.22%and the relative standard deviation were(RSDs)were 0.6%-4.8%.
关键词
化妆品/烯丙胺类/抗真菌类药物/超高效液相色谱-串联质谱法(UPLC-MS/MS)Key words
cosmetics/allylamine/antifungal drug/ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)引用本文复制引用
出版年
2024
NETL
NSTL
维普
万方数据