高效液相色谱-串联质谱法测定纺织品中的克莱范残留量  

Determination of Kelevan Residue in Textiles by High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：麦晓霞[1] 周长征[1] 兰丽丽[1] 廖建萌 徐敏[1] 曾丹丹 

机构地区：[1]广东出入境检验检疫技术中心,广东广州510623 [2]湛江市质量计量监督检测所,广东湛江524022

出　　处：《分析测试学报》2013年第9期1069-1074,共6页Journal of Instrumental Analysis

基　　金：国家检验检疫行业标准制定计划项目(2011B049);广东出入境检验检疫局科研项目(2009GDK55)

摘　　要：建立了高效液相色谱-串联质谱定量测定纺织品中克莱范（Kelevan）残留的分析方法。样品经甲醇-乙腈（1∶1）混合溶液超声提取，弗罗里硅柱净化，ESI负离子模式下多反应监测（MRM）模式测定。待测物经Hypersil GOLD C18色谱柱分离，以甲醇-5 mmol/L乙酸铵溶液为流动相进行梯度洗脱，外标法定量。结果显示，克莱范在1.0-200.0 μg/L 范围内线性关系良好，定量下限（以信噪比≥10计）为0.025 mg/kg，以0.025、0.250、0.625 mg/kg浓度进行加标后测得回收率为90.6%-103.4%，相对标准偏差为3.3%-5.2% 。本实验建立的方法简便、准确、可操作性强，弥补了国内纺织品中克莱范检测方法的空白。A high performance liquid chromatography-tandem mass spectrometric（LC-MS/MS） method was developed for the determination of kelevan residue in textiles.The sample was ultrasonically extracted with methanol-acetonitrile（1∶1） and the extract was purified with florisil column if necessary.The compound was separated on a Hypersil GOLD C18 column（100 mm×2.1 mm,5 μm） with 20% methanol-5 mmol/L ammonium acetate aqueous solution as mobile phase.The detection of kelevan was carried out by MS/MS with negative electrospray ionization under the multiple reaction monitoring mode using the external standard method.The calibration curve showed a good linearity in the range of 1.0-200.0 μg/L for the target compound.The limit of quantitation（S/N≥10） was 0.025 mg/kg.The recoveries of kelevan in cotton sample ranged from 90.6% to 103.4% at the spiked levels of 0.025,0.250,0.625 mg/kg with relative standard deviations（RSDs） of 3.3%-5.2%.With advantages of simplicity,accurancy and strong operability,the established method could be applied in the determination of kelevan in textiles.

关 键 词：克莱范 纺织品 液相色谱-串联质谱 

分 类 号：O657.63[理学—分析化学] F767.2[理学—化学]