加速溶剂萃取-固相萃取净化-GC/MS法测定纺织固废中16种多环芳烃  

Accelerated Solvent Extraction-Solid Phase Extraction Purification-GC/MS Method for the Determination of 16 Polycyclic Aromatic Hydrocarbons in Textile Solid Waste

作　　者：铁建成 刘俊 肖远淑[2] 贾丽霞[2] TIE Jian-cheng;LIU Jun;XIAO Yuan-shu;JIA Li-xia(CTC Nanjing Guocai Testing Limited Corporation,Nanjing 210046,China;College of Textiles and Clothing,Xinjiang University,Urumqi 830046,China;Urumqi Customs,Urumqi 830011,China;Chengdu Customs Technology Center,Chengdu 610041,China)

机构地区：[1]国检测试控股集团南京国材检测有限公司,江苏南京210046 [2]新疆大学纺织与服装学院,新疆乌鲁木齐830046 [3]乌鲁木齐海关,新疆乌鲁木齐830011 [4]成都海关技术中心,四川成都610041

出　　处：《化学试剂》2024年第8期99-106,共8页Chemical Reagents

基　　金：新疆维吾尔自治区重大科技专项项目(2020A03002-2)。

摘　　要：建立了加速溶剂萃取-固相萃取净化-气相色谱-质谱(ASE-SPE-GC/MS)的方法,用于纺织固体废物中16种多环芳烃(PAHs)的定性和定量分析。以丙酮-正己烷(V(丙酮)∶V(正己烷)=1∶1)作为萃取剂,采用L_(9)(3^(4))正交实验法对加速溶剂萃取条件进行选择和优化,提取液经MIP-PAHs固相萃取柱富集和净化,GC/MS进行测定,外标法定量。结果表明:16种PAHs在0.1~5 mg/L范围内线性良好,相关系数为0.9932~0.9998,检出限为0.82~1.95μg/kg,定量限为3.28~7.80μg/kg。在0.1、2、5 mg/L加标水平下,16种PAHs的回收率为73.7%~103.8%,日内相对标准偏差为0.7%~8.2%,日间相对标准偏差为1.4%~9.1%,满足分析检测的要求。ASE-SPE-GC/MS方法操作简便、干扰度低,适用于纺织固体废物中PAHs的检测分析。An accelerated solvent extraction-solid phase extraction purification-gas chromatography coupled with mass spectrometry(ASE-SPE-GC/MS)method was developed for the qualitative and quantitative analysis of 16 kinds of polycyclic aromatic hydrocarbons(PAHs)in textile solid waste.With acetone-n-hexane(V(acetone)∶V(n-hexane)=1∶1)as extractant,L_(9)(3^(4))orthogonal experiment was used to select and optimize the conditions of ASE.The extraction solution was enriched and purified by the MIP-PAHs solid-phase extraction column,determined by GC/MS and quantified by external standard method.The results showed that 16 PAHs had good linearity in the range of 0.1~5 mg/L with the correlation coefficients of 0.9932~0.9998,the detection limits were 0.82~1.95μg/kg,and the quantification limits were 3.28~7.80μg/kg.At the standard addition levels of 0.1,2 and 5 mg/L,the recoveries of 16 PAHs were 73.7%~103.8%,the intraday relative standard deviations(RSDs)were 0.7%~8.2%,and the daytime RSDs were 1.4%~9.1%,which met the requirements of analysis and detection.The ASE-SPE-GC/MS method is easy to operate and has low interference,which is suitable for the detection and analysis of PAHs in textile solid waste.

关 键 词：加速溶剂萃取 固相萃取净化 气相色谱-质谱法 纺织固体废物 多环芳烃 

分 类 号：O65[理学—分析化学]