超高效液相色谱-串联质谱法检测化妆品中二甲双胍的方法

Determination of Metformin in Cosmetics by UPLC-MS/MS

建立了一种化妆品中二甲双胍的超高效液相色谱-串联质谱(UPLC-MS/MS)分析检测方法。样品经过50%(体积分数)乙腈水溶液超声提取后,采用Waters Acquity UPLC BEH HILIC柱(150 mm×2.1 mm×1.7μm),以5 mmol/L乙酸铵溶液(含体积分数0.1%甲酸)和乙腈(含体积分数0.1%甲酸)为流动相进行梯度洗脱。质谱采用电喷雾离子源(ESI)、正离子扫描、多反应监测(MRM)模式进行检测。结果表明,在5~200 ng/L的质量浓度范围内,水基类、膏霜类、乳液类和面膜类4种基质化妆品中二甲双胍的线性关系均良好,相关系数(r)均大于0.995。检出限(LOD)为0.03~0.08μg/kg,定量限(LOQ)为0.10~0.25μg/kg。在3种质量浓度水平下的加标回收率为81.5%~118.2%,相对标准偏差(RSD)为3.8%~9.3%(n=6)。该方法具有简单、快速和灵敏度高等优点,适用于多种基质类化妆品中二甲双胍的测定。

A method was developed for determination of metformin in cosmetics by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The sample was ultrasonically extracted with 50%(in volume fraction)acetonitrile solution,then separated on a Waters Acquity UPLC BEH HILIC column(150 mm×2.1 mm×1.7μm)by gradient elution using 5 mmol/L ammonium acetate solution and acetonitrile both containing 0.1%(in volume fraction)formic acid as the mobile phases.The mass spectrometry was detected using electrospray ion source(ESI),positive ion scanning and multiple reaction monitoring(MRM)mode.The results showed that metformin had good linearity in the range of 5-200 ng/L with correlation coefficients(r)larger than 0.995 in toner,cream,emulsion and facial mask cosmetics.The limits of detection(LOD)were in the ranges of 0.03-0.08μg/kg and the limits of quantitation(LOQ)were in the ranges of 0.10-0.25μg/kg.The recoveries at 3 spiked levels for metformin in 4 types of matrix were 81.5%-118.2%with the relative standard deviations(RSD)of 3.8%-9.3%(n=6).With the advantages of simple,fast and high sensitivity,this method is suitable for the determination of metformin in various cosmetic matrices.