超高效液相色谱-串联质谱法同时测定祛痘类化妆品中保泰松与氨基比林的研究

摘要

建立了快速测定祛痘类化妆品中保泰松和氨基比林的固相萃取/超高效液相色谱-串联质谱分析方法.样品以乙腈为提取溶剂超声萃取,经Oasis HLB固相萃取柱净化浓缩后,采用Eclipse XDB-C18(3.5μm,4.6 mm×150 mm)色谱柱进行分离,甲醇-10 mmol·L-1乙酸铵溶液为流动相梯度洗脱,流速为0.5mL·min-1.采用电喷雾正离子源(ESI+),多反应监测(MRM)扫描方式检测,基质匹配标准曲线法定量.结果表明,保泰松和氨基比林在2.0～200.0 μg· L-范围内线性关系良好,相关系数(r2)均大于0.99,方法检出限分别为1.5、0.8μg.kg-1,定量下限分别为4.9、2.7μg· kg-1.低、中、高3个加标水平下的平均回收率为77.8％ ～ 93.4％,日内相对标准偏差(RSD)为2.4％～7.8％,日间RSD为3.6％ ～9.5％.该方法简捷、快速、检出限低,能够为化妆品中保泰松和氨基比林残留状况的监测工作和产品质量控制提供科学依据和技术支持.%An ultra performance liquid chromatography-tandem mass spectrometric (UPLC-MS/MS) method with solid phase extraction (SPE) was applied in the simultaneous determination of phenylbutazone and aminopyrine in anti-acne cosmetics.The sample was ultrasonically extracted with acetonitrile,and then purified on an Oasis HLB solid phase extraction column.The separation was performed with an Eclipse XDB-C18 (3.5 μm,4.6 mm × 150 mm) column,using a mixture of methanol and 10 mmol · L-1 ammonium acetate as mobile phase by gradient elution at a flow rate of 0.5 mL · min-1 The analytes were detected with electrospray ionization source in positive ion mode (ESI +) and multiple reaction monitoring (MRM),and quantified by matrix standard curve.The calibration curves of phenylbutazone and aminopyrine were linear in the range of 2.0-200.0 μg ·L-1 with correlation coefficients (r2) larger than 0.99.The limits of detection (LOD) and limits of quantitation(LOQ) of the method were 1.5,0.8 μg · kg-1 and 4.9,2.7 μg · kg-1,respectively.The recoveries of phenylbutazone and aminopyrine were in the range of 77.8％-93.4％ at three spiked levels,with intra-day and inter-day relative standard deviations(RSD) of 2.4％-7.8％ and 3.6％-9.5％,respectively.With fast detection,high sensitivity and low detection limit,the method is able to provide a scientific basis and a technical support for monitoring residues of phenylbutazone and aminopyrine in cosmetics and product quality control.