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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
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陈岑,黄柳倩,程巧鸳,周明昊,颜琳琦 浙江省食品药品检验研究院 
基金项目:浙江省食品药品监管系统科技计划项目(2019015)
中文摘要: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0.22 μm滤膜上机检测。采用XSelect CSH C18色谱柱(2.1 mm×150 mm,3.5 μm)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5~500 μg/L范围内线性良好,相关系数(r2)>0.99,检出限(LOD)和定量下限(LOQ)分别为0.8~200 μg/kg和4~400 μg/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。
中文关键词:QuEChERS  硝基咪唑类(NMZs)  高效液相色谱-串联质谱法(HPLC-MS/MS)  化妆品  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
Abstract: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 0.22 μm microporous membrane.The target compounds were separated on an XSelect CSH C18(2.1 mm×150 mm,3.5 μm) 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 5-500 μg/L with their correlation coefficients(r2) all above 0.99.The limits of detection(LOD) and limits of quantitation(LOQ) were in the ranges of 0.8-200 μg/kg and 4-400 μg/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.
Key Words:QuEChERS  nitroimidazoles(NMZs)  high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)  cosmetics  prohibited drugs
引用本文:陈岑,黄柳倩,程巧鸳,周明昊,颜琳琦.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[J].分析测试学报,2019,38(11):1285-1293.
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