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作 者:刘轩彤 王天歌 赵迎春 LIU Xuantong;WANG Tiange;ZHAO Yingchun(Shenyang Food and Drug Inspection Institute,Shenyang 110000,Liaoning,China)
出 处:《香料香精化妆品》2024年第2期188-192,共5页Flavour Fragrance Cosmetics
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×1.7μm)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%。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×1.7μm)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%.
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