超高效液相色谱-串联质谱测定婴幼儿纺织用品中的喹啉和异喹啉残留量  

Determination of Quinoline and Isoquinoline in Textile Products for Infants by Ultra-high Performance Fast Liquid Chromatography-Tandem Mass Spectrometry

作　　者：李志刚[1] 蒋少军[1] 戴鸽 LI Zhigang;JIANG Shaojun;DAI Ge(Jian HU Branch of Zhejiang Industry Polytechnic College,Shaoxing 312000;Ningbo Shenzhou Knitting Co.,Ltd.,Ningbo 315000)

机构地区：[1]浙江工业职业技术学院鉴湖学院,浙江绍兴312000 [2]宁波申洲针织有限公司,浙江宁波315000

出　　处：《分析科学学报》2022年第3期339-344,共6页Journal of Analytical Science

摘　　要：利用分散固相萃取,结合超快速液相色谱-串联质谱技术,建立了婴幼儿纺织用品中喹啉和异喹啉残留量的检测方法。样品经甲醇提取,提取液用SCX吸附剂净化后,氮气吹干,流动相复溶,采用Acquity UPLC BEH C18柱,以乙腈/水溶液(体积比5∶95,含0.1%甲酸)为流动相,等度洗脱,电喷雾正离子模式电离,多反应监测模式检测,外标法定量。喹啉和异喹啉在0.5~100μg/mL范围内线性关系良好,它们的检出限为0.16μg/kg,定量限为0.5μg/kg;添加浓度分别为1.0、5.0、50.0μg/kg时,喹啉和异喹啉的加标回收率分别为90.2%~104.5%和91.6%~105.6%,相对标准偏差分别为2.4%~5.3%和3.8%~6.3%。该方法简单、快速、灵敏度高,稳定性好,能够满足婴幼儿纺织用品中喹啉和异喹啉的检测要求。A novel method has been developed for rapid separation and determination of quinoline and isoquinoline in textile products for infants by dispersive solid phase extraction(dSPE)coupled with ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The target compounds in textile products were extracted by MeOH.The extract was purified by SCX.The extracts were blowed with N_(2) to nearly dry,and redissolved in the solvent of acetonitrile and water(5∶95 V/V,including 0.1%formic acid).The chromatographic analysis was performed on an Acquity UPLC BEH C18 column by an isocratic elution employing acetonitrile and water(5∶95 V/V,including 0.1%formic acid)as a mobile phase.The analytes were detected by electrospray onization(ESI)tandem mass spectrometry with multiple reaction monitoring(MRM)in positive ion mode.The calibration curves showed good linearity in the range of 0.5-100μg/mL for quinoline and isoquinoline with the limits of detection of 0.16μg/kg and the limits of quantification of 0.5μg/kg.The recoveries of quinoline and isoquinoline in textile products for infants at the spiked concentration levels of 1.0,5.0 and 50.0μg/kg ranged from 90.2%to 104.5%and from 91.6%to 105.6%,respectively.Relative standard deviations were between 2.4%-5.3%and 3.8%-6.3%(n=6).The method is highly sensitive and accurate,and is suitable for the analysis of quinoline and isoquinoline in textile products for infants.

关 键 词：超快速液相色谱-串联质谱 婴幼儿纺织用品 喹啉 异喹啉 

分 类 号：O657.63[理学—分析化学]