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

引用本文: 魏丹, 国明, 吴慧珍, 张菊. 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[J]. 色谱, 2020, 38(8): 945-952. doi: 10.3724/SP.J.1123.2019.12028 shu

Citation: WEI Dan, GUO Ming, WU Huizhen, ZHANG Ju. 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[J]. Chinese Journal of Chromatography, 2020, 38(8): 945-952. doi: 10.3724/SP.J.1123.2019.12028 shu

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.
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

通讯作者: 魏丹, E-mail:1422547228@qq.com

基金项目:
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）.

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:

English

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 Dan ^{1,
,} ,
GUO Ming ^2, ,
WU Huizhen ^3, ,
ZHANG Ju ^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

Corresponding author: WEI Dan, 1422547228@qq.com

Received Date: 20 December 2019
Fund Project:
the Scientific Research Project of the Zhejiang Provincial Education Department (No. Y201840776)

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

1. [1] Lammel G, Sehili A M, Bond T C, et al. Chemosphere, 2009, 76(1): 98
2. [2] Atmaca E, Das Y K, Yavuz O, et al. Environ Sci and Pollut R, 2019, 26(7): 7005
3. [3] Zhang P, Chen Y G. Sci Total Environ, 2017, 605/606: 1011
4. [4] Balcioglu E B. Toxin Rev, 2016, 35(3/4): 98
5. [5] Marsin F M, Wan I, Wan A, et al. J Chromatogr A, 2019, 1612: 460638
6. [6] Sun Y Q, Wu S M. Food Control, 2020, 109: 106950
7. [7] Cardenas-Soraca D M, Tucca F I, Mardones-Pena C A. J Chromatogr A, 2019, 1605: 360341
8. [8] Mona K, Souaya E R, Hamzawy A H, et al. Int J Anal Chem, 2015, 2015: 1
9. [9] Song X J, He X R, Yin M M, et al. Chinese Journal of Chromatography, 2018, 36(10): 1038 宋晓娟, 贺心然, 尹明明, 等. 色谱, 2018, 36(10): 1038
10. [10] Rimayi C, Chimuka L. Environ Monit Assess, 2019, 191(11): 700
11. [11] Tan J, Lu X B, Fu L, et al. Ecotox Environ Saf, 186: 109775
12. [12] Fu H, Hu X J, Chen X, et al. Chinese Journal of Chromatography, 2018, 36(5): 487 付慧, 胡小键, 陈曦, 等. 色谱, 2018, 36(5): 487
13. [13] Nian Q X, Liu Y M, Sun B, et al. Chinese Journal of Chromatography, 2019, 37(3): 252 念琪循, 刘园满, 孙冰, 等. 色谱, 2019, 37(3): 252
14. [14] Brandl R C, Bucheli T D, Kupper T, et al. Int J Environ Anal Chem, 2006, 86(7): 505
15. [15] Huang W, Li N, Xu R H, et al. Chinese Journal of Chromatography, 2018, 36(12): 1303 黄微, 李娜, 徐瑞晗, 等. 色谱, 2018, 36(12): 1303
16. [16] Si X X, Lu S M, Liu Z H, et al. Chinese Journal of Chromatography, 2016, 34(3): 340 司晓喜, 陆舍铭, 刘志华, 等. 色谱, 2016, 34(3): 340
17. [17] Huang L J, He M, Chen B B, et al. Chemosphere, 2018, 199: 435
18. [18] Zhang W M, Yan Z M, Gao J, et al. J Chromatogr A, 2015, 1400: 10
19. [19] Chen X F, Ding N, Zang H, et al. J Chromatogr A, 2013, 1304: 241
20. [20] Li J, Wu Y N, Li Z, et al. J Phys Chem C, 2014, 118(47): 27382
21. [21] Gee J A, Chung J, Nair S, et al. J Phys Chem C, 2016, 117(6): 3169
22. [22] Liu X M, Sun Z W, Chen G, et al. J Chromatogr A, 2015, 1409: 46
23. [23] Hong B. [MS Dissertation]. Shenyang: Liaoning University, 2016 洪保. [硕士学位论文]. 沈阳: 辽宁大学, 2016
24. [24] HJ 835-2017
25. [25] HJ 805-2016

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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

通讯作者: 魏丹, E-mail:1422547228@qq.com

English

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

Corresponding author: WEI Dan, 1422547228@qq.com

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

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

通讯作者: 魏丹, E-mail:1422547228@qq.com

English

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

Corresponding author: WEI Dan, 1422547228@qq.com

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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