基于QuEChERS提取的高效液相色谱-串联质谱法同时测定4种不同基质类型化妆品中15种硝基咪唑类禁用药物

Simultaneous Determination of 15 Prohibited Nitroimidazoles in 4 Matrixes of Cosmetics by High Performance Liquid Chromatography-Tandem Mass Spectrometry with QuEChERS Extraction

建立了同时测定4种不同基质类型化妆品中15种硝基咪唑类(NMZs)禁用药物的高效液相色谱-串联质谱法(HPLC-MS/MS)。样品经溶剂超声提取,改良的QuEChERS方法净化后,过0.22μm滤膜上机检测。采用XSelect CSH C18色谱柱(2.1 mm×150 mm,3.5μm)进行分离,以0.1%甲酸乙腈-0.1%甲酸水溶液作为流动相梯度洗脱,流速为0.25 mL/min。采用正离子模式电喷雾电离(ESI+),多反应监测(MRM)模式检测,基质匹配标准曲线外标法定量。结果表明,15种硝基咪唑类药物在5~500μg/L范围内线性良好,相关系数(r^2)>0.99,检出限(LOD)和定量下限(LOQ)分别为0.8~200μg/kg和4~400μg/kg。3个不同浓度加标水平下,平均加标回收率为86.8%~115%,相对标准偏差(RSD)为0.3%~8.4%。该方法前处理简单、分离效果好、回收率高,适用于化妆品中硝基咪唑类禁用药物的测定。

A high performance liquid chromatography-tandem mass spectrometric(HPLC-MS/MS)method was developed for the simultaneous determination of 15 prohibited nitroimidazoles(NMZs)in 4 matrixes of cosmetics.Samples were ultrasonically extracted with solvent,and then purified by modified QuEChERS method,filtered through a 0.22μm microporous membrane.The target compounds were separated on an XSelect CSH C 18(2.1 mm×150 mm,3.5μm)column by gradient elution using acetonitrile solution containing 0.1%formic acid-0.1%formic acid as mobile phase at a flow rate of 0.25 mL/min.The MS/MS analysis was performed with electrospray ion source in positive mode under multiple reaction monitoring(MRM)mode.The matrix-matched calibration was used for the quantification.Results showed that there were good linear relationships for 15 nitroimidazoles in the concentration range of 5-500μg/L with their correlation coefficients(r 2)all above 0.99.The limits of detection(LOD)and limits of quantitation(LOQ)were in the ranges of 0.8-200μg/kg and 4-400μg/kg,respectively.The recoveries for 15 prohibited drugs at three spiked levels were in the range of 86.8%-115%with relative standard deviations(RSD)of 0.3%-8.4%.With simple pretreatment,high separation efficiency and high recovery,the method was suitable for the analysis of nitroimidazoles in cosmetics products.