色谱 ›› 2020, Vol. 38 ›› Issue (8): 945-952.DOI: 10.3724/SP.J.1123.2019.12028

• 研究论文 • 上一篇    下一篇

加速溶剂萃取-磁固相萃取净化-气相色谱-质谱法测定土壤中16种多环芳烃和23种有机氯残留

魏丹1,*(), 国明2, 吴慧珍3, 张菊1   

  1. 1 河北经贸大学生物科学与工程学院, 河北 石家庄 050061
    2 浙江省化工研究院有限公司 分析测试中心, 浙江 杭州 310023
    3 浙江树人大学生物与环境工程学院, 浙江 杭州 310015
  • 收稿日期:2019-12-20 出版日期:2020-08-08 发布日期:2020-12-11
  • 通讯作者: 魏丹
  • 作者简介:魏丹.Tel:(0311)87655680, E-mail:1422547228@qq.com
  • 基金资助:
    浙江省教育厅一般科研项目(Y201840776);浙江省分析测试项目(2018C37047);河北经贸大学科研基金项目(2017KYZ05)

Determination of 16 polycyclic aromatic hydrocarbon and 23 organochlorine residues in soil by accelerated solvent extraction and magnetic solid phase purification- gas chromatography-tandem mass spectrometry

WEI Dan1,*(), GUO Ming2, WU Huizhen3, ZHANG Ju1   

  1. 1 College of Bioscience and Engineering, Hebei University of Economics and Business; Shijiazhuang 050061, China
    2 Center of Analysis and Testing, Zhejiang Research Institute of Chemical Industry Co., Ltd., Hangzhou 310023, China
    3 College of Biological and Environmental Engineering, Zhejiang Shuren University, Hangzhou 310015, China
  • Received:2019-12-20 Online:2020-08-08 Published:2020-12-11
  • Contact: WEI Dan
  • Supported by:
    the Scientific Research Project of the Zhejiang Provincial Education Department(Y201840776);the Analysis Test Project of Zhejiang Province(2018C37047);the Project of Scientific Research Foundation of Hebei University of Economics and Business(2017KYZ05)

摘要:

建立了加速溶剂萃取(ASE)、磁固相萃取净化(MSPE)、气相色谱-质谱(GC-MS)测定土壤中多环芳烃和有机氯残留的方法。ASE萃取溶剂为丙酮-正己烷(1:1,v/v),萃取温度为100℃,萃取压力为11.032 MPa,加热时间为5 min,静态萃取时间为5 min,循环萃取3次,冲洗体积为60%萃取池体积,氮气吹扫100 s。然后采用室温制备法自制ZIF-8/nZVI磁性材料用于净化萃取液,将净化液浓缩定容后进行GC-MS测定。多环芳烃和有机氯的线性范围为5~200 μg/kg,线性相关系数(r2)均大于0.99;目标物的检出限(LOD,S/N=3)为0.04~1.21 μg/kg。所建方法成功用于土壤样品中16种多环芳烃和23种有机氯的测定,在3个加标水平下得到的加标回收率为63.9%~112.1%,相对标准偏差(RSD)为0.4%~26.2%。研究结果表明,该方法具有灵敏度高、重现性好、回收率高等特点,适用于土壤中多环芳烃和有机氯残留的检测。

关键词: 气相色谱-串联质谱, 加速溶剂萃取, 磁固相萃取, 多环芳烃, 有机氯, 土壤

Abstract:

A method combining accelerated solvent extraction (ASE) with magnetic solid-phase extraction (MSPE) and gas chromatography-mass spectrometry (GC-MS) was developed for the simultaneous detection of polycyclic aromatic hydrocarbon (PAH) and organochlorinepesticide (OCP) residues in soil samples. The analytes in the soil samples were extracted using an acetone/n-hexane (1:1, v/v) mixture for 5 min at 100℃. Then, the extraction pool was heated for 5 min under an extractive pressure of 11.032 MPa for three cycles. The extraction pool was washed with an acetone/n-hexane (1:1, v/v) mixture accounting for 60% of the pool volume, followed by nitrogen purging for 100 s. The extract was purified by MSPE using self-made magnetic ZIF-8/nZVI materials at room temperature. The analytes were detected by GC-MS/MS. Under the optimized conditions, good linearities were obtained for the 16 PAHs and the 23 OCPs in the range of 5-200 μg/kg, with correlation coefficients (r2) above 0.99. The limits of detection (LODs) were 0.04-1.21 μg/kg. At three spiked levels in the soil samples, the recoveries of the 39 analytes were between 63.9% and 112.1%, with relative standard deviations (RSDs) between 0.4% and 26.2%. The method was demonstrated to be successful for the determination of 16 PAH and 23 OCP residues in soil samples, with good recoveries.

Key words: gas chromatography-mass spectrometry (GC-MS), accelerated solvent extraction (ASE), magnetic solid-phase extraction (MSPE), polycyclic aromatic hydrocarbon (PAH), organochlorine pesticide (OCP), soil samples