分析测试学报2017,Vol.36Issue(8):980-985,6.DOI:10.3969/j.issn.1004-4957.2017.08.006
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
Simultaneous Determination of Phenylbutazone and Aminopyrine in Anti-acne Cosmetics by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
摘要
Abstract
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.关键词
超高效液相色谱-串联质谱/化妆品/保泰松/氨基比林/固相萃取Key words
ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)/cosmetics/phenylbutazone/aminopyrine/solid phase extraction (SPE)分类
化学化工引用本文复制引用
熊爽,刘成雁,王志嘉,李红,任雪冬,王璐,田福林,赵海波..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[J].分析测试学报,2017,36(8):980-985,6.基金项目
国家重大科学仪器设备开发专项资助(2012YQ1200440602) (2012YQ1200440602)
辽宁省科学事业公益研究基金项目资助(2014002001) (2014002001)