【摘要】 利用超高效液相色谱-串联质谱(UPLC-MS/MS)结合凝胶渗透色谱(GPC)技术,建立了一种快速分离和测定皮革制品中7种尼泊金酯类防腐剂的分析方法。样品经超声提取、浓缩、GPC净化,甲醇-水溶液(1∶1,v/v)溶解,采用Acquity UPLCBEH C18柱(50 mm×2.1 mm,1.7μm)分离,以甲醇和水为流动相,梯度洗脱,电喷雾负离子模式电离,采用多反应监测模式检测和外标法定量。该方法在0.1～1.0 mg/L范围内线性关系良好(r>0.99);在添加量为0.5～3.0 mg/kg时,平均回收率为(79.44±5.67)%～(98.07±9.50)%,相对标准偏差(RSD)为4.24%～14.00%;方法的检出限(LOD)为4～12μg/kg,定量限(LOQ)为13.2～39.6μg/kg。该方法操作简便、快捷、灵敏、准确,适合皮革中多种尼泊金酯类防腐剂的确证和定量测定。更多还原

【Abstract】 A novel method has been developed for the rapid separation and determination of 7 nipagin ester preservatives in leather by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) coupled with gel permeation chromatographic(GPC) clean-up.Nipagin ester preservatives in leather were extracted by ultrasonic extraction with methanol.The extract was dried by a rotavapor and purified by GPC,then redissolved in the solvent of methanol-water(1∶1,v/v).The chromatographic analysis was performed on an Acquity UPLC BEH C18 column(50 mm×2.1 mm,1.7 μm) with a gradient elution of methanol and water as the mobile phases.The analytes were detected by electrospray ionization(ESI) tandem mass spectrometry with multiple reaction monitoring(MRM) in negative ion mode.Good linearity(r> 0.99) was observed between 0.1 and 1.0 mg/L for all the analytes.The recoveries and relative standard deviations(RSDs) were checked by spiking samples with the 7 nipagin ester preservatives at the three levels of 0.5,1.0 and 3.0 mg/kg.The average recoveries of the 7 nipagin ester preservatives were from(79.44±5.67)% to(98.07±9.50)%.The precision values expressed as RSD ranged from 4.24% to 14.00%(n=6).The limits of detection were 4-12 μg/kg and the limits of quantification were 13.2-39.6 μg/kg for the analytes.The method is simple,rapid,sensitive and accurate,and suitable for the quantitative determination and confirmation of 7 nipagin ester preservatives in leather.更多还原