加速溶剂萃取/气相色谱-三重四极杆串联质谱法测定纺织品中24种多环芳烃  

Determination of 24 Polycyclic Aromatic Hydrocarbons in Textiles by Gas Chromatography-Triple Quadrupole Mass Spectrometry with Accelerated Solvent Extraction

作　　者：裴德君 连秋燕 刘贵 朱峰 陈金泉 杨瑜榕 PEI De-jun;LIAN Qiu-yan;LIU Gui;ZHU Feng;CHEN Jin-quan;YANG Yu-rong(National Textile and Garment Quality Supervision Testing Center(Fujian),Fuzhou 350026,China;Fujian Key Laboratory of Textiles Inspection Technology,Fuzhou 350026,China)

机构地区：[1]国家纺织服装产品质量监督检验中心,福建福州350026 [2]福建省纺织产品检测技术重点实验室,福建福州350026

出　　处：《分析测试学报》2018年第8期940-944,共5页Journal of Instrumental Analysis

基　　金：福建省自然科学基金项目(2016J05025)

摘　　要：建立了加速溶剂萃取/气相色谱-三重四极杆串联质谱(ASE/GC-MS/MS)同时测定纺织品中24种多环芳烃(PAHs)的方法。样品经丙酮加速溶剂萃取,旋蒸浓缩后采用DB-35色谱柱程序升温分离,选择多反应监测模式(MRM)采集,外标法定量。结果表明,在一定浓度范围内多环芳烃的峰面积与质量浓度呈良好的线性关系,相关系数(r^2)均大于0.994,方法检出限为0.000 3~0.03 mg/kg,方法定量下限为0.001~0.10 mg/kg,加标回收率为80.3%~103%,相对标准偏差(RSD)为1.3%~9.2%。该方法灵敏、准确可靠,能满足纺织品中24种多环芳烃的测试要求。An analytical method based on gas chromatography-triple quadrupole mass spectrometry with accelerated solvent extraction(ASE/GC-MS/MS)was established for the simultaneous determination of 24 polycyclic aromatic hydrocarbons(PAHs)in textiles.PAHs in the samples were extracted by ASE with acetone,and evaporated to dryness with a rotary evaporator.The separation was performed on a DB-35 capillary column by temperature programming.The identification was performed by GC-MS/MS in multiple reaction monitoring(MRM)mode,and the quantitation was carried out by the external standard method.The calibration curves for 24 PAHs showed good linearities in the certain concentration with correlation coefficients(r 2)larger than 0.994.The limits of detection(LODs)and quantitation(LOQs)for PAHs in textiles were in the ranges of 0.000 3-0.03 mg/kg and 0.001-0.10 mg/kg,respectively.The average recoveries were in the range of 80.3%-103%with relative standard deviations(RSDs,n=6)of 1.3%-9.2%.The method is suitable for the simultaneous determination of 24 PAHs in textiles with high sensitivity,accuracy and reliability.

关 键 词：气相色谱-三重四极杆串联质谱法(GC-MS/MS) 加速溶剂萃取(ASE) 纺织品 多环芳烃 

分 类 号：O657.63[理学—分析化学] O625.15[理学—化学]