高效液相色谱-串联质谱法同时测定化妆品中5种皮肤外用药

Simultaneous determination of five topical dermatological drugs in cosmetics by ultra-performance liquid chromatography-tandem mass spectrometry

建立了高效液相色谱-串联质谱法同时测定化妆品中莫匹罗星、特比萘芬、夫西地酸、红霉素、噻吗洛尔5种皮肤外用药的检测方法。样品采用80%乙腈超声提取,以0.1%的甲酸水溶液和乙腈为流动相,梯度洗脱,经C18(2.1 mm×50 mm,1.9µm)色谱柱分离后,采用电喷雾电离源(ESI),在正、负离子多反应监测(MRM)扫描模式下进行定性定量分析。结果显示,5种禁用原料在各自范围线性关系良好,相关系数均在0.995以上;方法检出限为0.001~0.02 mg/kg,定量限为0.003~0.06 mg/kg,在膏霜、乳液、水剂3种基质中平均加标回收率为79.6%~102.4%,相对标准偏差为1.2%~6.6%(n=6)。该方法特异性强、灵敏度高、精密度好,操作简便,可用于化妆品中5种皮肤外用药的定性定量测定。

An analytical method for simultaneous determination of five topical dermatological drugs,including mupirocin,terbinafine,fusidine,erythromycin and timolol,in cosmetics was established by ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The cosmetic samples were ultrasonically extracted with the mixed solvent of 80%acetonitrile-water.The gradient elution was carried out with 0.1%formic acid aqueous solution-acetonitrile as mobile phase.The components in the purified extract were separated on the C18(2.1 mm×50 mm,1.9μm)column and then detected by mass spectrometry.The qualitative and quantitative analysis of the five prohibited substances was performed using electrospray ionization(ESI)in positive and negative ion mode with the multiple reaction monitoring(MRM).The results show that the five prohibited substances have good linear relationship in their respective concentration range,with the correlation coefficients(r)more than 0.995.The limits of detection are in the range of 0.001~0.02 mg/kg and the limits of quantification are in the range of 0.003~0.06 mg/kg.The average recoveries in sample matrix of cream,emulsion and water are 79.6%~102.4%,while the relative standard deviations(n=6)are 1.2%~6.6%.This method is specific,sensitive,accurate and simple to operate,which is available for qualitative and quantitative analysis of the five common topical dermatological drugs in cosmetics.