【摘要】 利用超高效液相色谱串联四极杆质谱(UPLC-MS/MS)联用技术,建立一种能在7 min内快速分离和测定纺织品中7种尼泊金酯类防腐剂的方法。样品经超声提取、浓缩,甲醇-水(体积比为1∶1)溶解,采用Acquity UPLCBEH C18液相色谱柱,以甲醇水溶液为流动相,梯度洗脱,电喷雾负离子模式电离,多反应监测模式检测,外标法定量。该方法检出限(LOD)为4～12μg/kg;在0.1～1.0μg/mL范围内线性关系良好,添加量分别为0.5、1.0、3.0 mg/kg时,添加回收率范围为(76.09±4.92)%～(106.65±4.90)%,相对标准偏差为4.60%～14.88%。更多还原

【Abstract】 A novel method has been developed for rapid separation and determination of 7 nipagin esters in textiles by ultrahigh performance liquid chromatography-mass spectrometry(UPLC-MS/MS) within 7 min.Nipagin esters residues in textiles were extracted by ultrasonic extraction with methanol.The extract was concentrated and redissolved in the mixed solvent of methanol and water(volume ratio of 1∶1).The chromatographic analysis was performed on an Acquity UPLC BEH C18 column by a gradient elution employing methanol and water as a mobile phase.Electrospray ionization(ESI) was conducted in negative ion mode;detection was undertaken with multiple reaction monitoring(MRM);and external standard was used for quantitative determination.The calibration curves showed good linearity in the range of 0.1-1.0 μg/mL for all nipagin esters with the limits of determination(LOD) of 4-12 μg/kg.The recoveries of 7 nipagin esters at the spiked concentration levels of 0.5,1.0 and 3.0 mg/kg ranged from(76.09 ± 4.92)% to(106.65 ± 4.90)% with relative standard deviations(RSDs) of 4.60%-14.88%.更多还原