Simultaneous determination of multiple persistent organic pollutants in soil by ultrasonic extract-gas chromatography-mass spectrometry

doi:10.3785/j.issn.1008-9209.2021.04.072

Journal of Zhejiang University (Agriculture and Life Sciences)

2022, Vol. 48

Issue (3): 336-350 DOI: 10.3785/j.issn.1008-9209.2021.04.072

Resource utilization & environmental protection

Simultaneous determination of multiple persistent organic pollutants in soil by ultrasonic extract-gas chromatography-mass spectrometry

Hao ZHANG¹(

),Ronglang HUANG²,Minyan CHEN²,Jun JIANG²,Lan YANG¹,Jian CHEN³,Zhijiang Lü¹,Min LIAO¹,Haizhen WANG¹(

),Jianming XU¹

^1.Zhejiang Provincial Key Laboratory of Agricultural Resources and Environment, College of Environmental and Resource Sciences, Zhejiang University, Hangzhou 310058, China
^2.Hangzhou Service Quality Testing Technology Co. , Ltd. , Hangzhou 311300, China
^3.Bureau of Agriculture and Rural Affairs and Water Resource of Wenling, Taizhou 317500, Zhejiang, China

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Abstract

A method for simultaneous extraction, purification, and determination of persistent organic pollutants (POPs) in soil, such as polychlorinated biphenyls, polybrominated diphenyl ethers, and polycyclic aromatic hydrocarbons, was developed in this study. The optimum conditions for extraction and purification were as follows: Soil samples were extracted ultrasonically three times with acetone/n-hexane (1∶?1, by volume), followed by purification with Florisil solid-phase extraction column, and eluted by 12 mL of n-hexane/dichloromethane (9∶1, by volume) mixture solution. The eluant was concentrated by gentle N₂ streams and finally quantified by gas chromatography-mass spectrometry (GC-MS) with PCB209 as the internal standard. Except for 2, 2′, 3, 3′, 4, 4′, 5, 5′, 6, 6′-decabromodiphenyl ether (BDE209), the other 41 POPs were efficiently separated within 23.83 min. Excellent linearity was observed in the concentration range of 20-1 000 μg/L for all POPs with the coefficients of determination (R²) of 0.997 5-0.999 9. The detection limits of 42 POPs were 0.04-1.19 ng/g, and the spiked recoveries ranged from 71.04% to 120.89% with relative standard deviations of 0.88%-6.29%, and intra- and inter-day reproducibility variations were less than 11%. In conclusion, this method greatly reduces time and workload and is characterized by simple operation, good accuracy, and high sensitivity. It can be widely applied to the determination and analysis of POPs in soil, such as e-waste disposal site soil, which will facilitate further studies on the fate and risk assessment of POPs.

Key words： polychlorinated biphenyls polybrominated diphenyl ethers polycyclic aromatic hydrocarbons ultrasonic extract solid phase extraction purification gas chromatography-mass spectrometry

Received: 07 April 2021 Published: 07 July 2022

CLC:

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Corresponding Authors: Haizhen WANG E-mail: 21914148@zju.edu.cn;wanghz@zju.edu.cn

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	Hao ZHANG
	Ronglang HUANG
	Minyan CHEN
	Jun JIANG
	Lan YANG
	Jian CHEN
	Zhijiang Lü
	Min LIAO
	Haizhen WANG
	Jianming XU

Cite this article:

Hao ZHANG,Ronglang HUANG,Minyan CHEN,Jun JIANG,Lan YANG,Jian CHEN,Zhijiang Lü,Min LIAO,Haizhen WANG,Jianming XU. Simultaneous determination of multiple persistent organic pollutants in soil by ultrasonic extract-gas chromatography-mass spectrometry. Journal of Zhejiang University (Agriculture and Life Sciences), 2022, 48(3): 336-350.

URL:

https://www.zjujournals.com/agr/10.3785/j.issn.1008-9209.2021.04.072 OR https://www.zjujournals.com/agr/Y2022/V48/I3/336

超声提取-气相色谱-质谱法对土壤中多种类持久性有机污染物的同时测定

本研究建立了同时提取、同时净化、同时测定土壤中多氯联苯、多溴二苯醚和多环芳烃等多种类持久性有机污染物（persistent organic pollutants, POPs）的方法，其提取和净化的最佳条件为：以V（丙酮）∶V（正己烷）=1∶1的混合溶液作为提取溶剂，超声提取3次；净化小柱为弗罗里硅土固相萃取柱；以V（正己烷）∶V（二氯甲烷）=9∶1的混合溶液作为洗脱溶剂，用量12 mL。经氮吹浓缩后，利用气相色谱-质谱联用法测定，内标法定量。结果表明：除2，2′，3，3′，4，4′，5，5′，6，6′-十溴二苯醚（BDE209）外，其余41种POPs仅在23.83 min内就得到很好的分离。42种目标POPs均在20～1 000 μg/L范围内线性关系良好，决定系数（R²）为0.997 5～0.999 9；方法的检出限为0.04～1.19 ng/g，加标回收率为71.04%～120.89%，相对标准偏差为0.88%～6.29%，日内重复性和日间重现性变化均小于11%。该方法大大减少了检测时间和工作量，并且操作简单、准确性好、灵敏度高，可大规模应用于废旧电器拆解场地等的土壤样品中POPs的测定分析，对POPs的检测及其环境行为研究等具有重要意义。

关键词： 多氯联苯, 多溴二苯醚, 多环芳烃, 超声提取, 固相萃取净化, 气相色谱-质谱联用

峰号 Peak number	持久性有机污染物 Persistent organic pollutant	保留时间 Retention time/min	定性离子 Qualitative ion (m/z)	定量离子 Quantitative ion (m/z)
1	萘 NAP	7.458	128，127，129	128
2	苊烯 ANY	9.396	152，151，153	152
3	苊 ANA	9.615	154，153，152	154
4	芴 FLU	10.238	166，165，167	166
5	菲 PHE	11.398	178，179，176	178
6	蒽 ANT	11.462	178，179，176	178
7	2，4，4′-三氯联苯 PCB28	11.851	256，258，186	256
8	2，2′，5，5′-四氯联苯 PCB52	12.186	292，290，220	292
9	荧蒽 FLT	12.863	202，200，203，101，100	202
10	2，2′，4，5，5′-五氯联苯 PCB101	13.056	326，328，254	326
11	芘 PYR	13.136	202，200，203，101，100	202
12	3，4，4′，5-四氯联苯 PCB81	13.348	292，290，220	292
13	3，3′，4，4′-四氯联苯 PCB77	13.453	292，290，220	292
14	2′，3，4，4′，5-五氯联苯 PCB123	13.685	326，328，254	326
15	2，3′，4，4′，5-五氯联苯 PCB118	13.709	326，328，254	326
16	2，4，4′-三溴二苯醚 BDE28	13.747	407.8，405.8，403.8	407.8
17	2，3，4，4′，5-五氯联苯 PCB114	13.843	326，328，254	326
18	2，2′，4，4′，5，5′-六氯联苯 PCB153	13.946	360，362，290	360
19	2，3，3′，4，4′-五氯联苯 PCB105	14.018	326，328，254	326
20	2，2′，3，4，4′，5′-六氯联苯 PCB138	14.282	360，362，290	360
21	3，3′，4，4′，5-五氯联苯 PCB126	14.396	326，328，254	326
22	2，3′，4，4′，5，5′-六氯联苯 PCB167	14.611	360，362，290	360
23	苯并（a）蒽 BaA	14.899	228，226，229，114，113	228
24	2，3，3，4，4′，5′-六氯联苯 PCB156	14.921	360，362，290	360
25	? CHR	14.971	228，226，229，114，113	228
26	2，3，3′，4，4′，5′-六氯联苯 PCB157	14.992	360，362，290	360
27	2，2′，3，4，4′，5，5′-七氯联苯 PCB180	15.124	394，396，324	394
28	2，2′，4，4′-四溴二苯醚 BDE47	15.207	485.8，483.8，487.8	485.8
29	3，3′，4，4′，5，5′-六氯联苯 PCB169	15.433	360，362，288	360
30	2，3，3′，4，4′，5，5′-七氯联苯 PCB189	15.960	394，396，324	394
31	2，2′，4，4′，6-五溴二苯醚 BDE100	16.531	565.7，563.7，561.7	565.7
32	2，2′，4，4′，5-五溴二苯醚 BDE99	16.920	565.7，563.7，561.7	565.7
33	苯并（b）荧蒽 BbFA	16.944	252，253，250，251	252
34	苯并（k）荧蒽 BkFA	16.993	252，253，250，251	252
35	苯并（a）芘 BaP	17.574	252，253，250，251	252
36	2，2′，4，4′，5，6′-六溴二苯醚 BDE154	18.100	643.6，641.6，645.6	643.6
37	2，2′，4，4′，5，5′-六溴二苯醚 BDE153	18.663	643.6，641.6，645.6	643.6
38	茚并（1，2，3-cd）芘 IPY	19.653	276，277，275，274	276
39	二苯并（a，h）蒽 DBA	19.700	278，276，279，138	278
40	苯并（g，h，i）苝 BPE	20.091	276，275，274，138	276
41	2，2′，3，4，4′，5′，6-七溴二苯醚 BDE183	20.449	721.6，719.6，563.6	721.6
42	2，2′，3，3′，4，4′，5，5′，6，6′-十溴二苯醚 BDE209	10.843	799.4，797.4，795.4	799.4

Table 1 Retention time, qualitative and quantitative ions of 42 persistent organic pollutants (PCBs, PBDEs, PAHs)

Fig. 1 Total ion chromatograms of 41 persistent organic pollutants (A) and BDE209 (B) in the standard samples

Fig. 2 Effects of different extraction methods on the recoveries of PCBs (A), PBDEs (B) and PAHs (C) in soilPlease see the Table 1 for details of the names of pollutants represented by abbreviations, and the same as below.

Fig. 3 Effects of different purification SPE columns on the recoveries of PCBs (A), PBDEs (B) and PAHs (C) in soil

Fig. 4 Effects of different elution solvents on the recoveries of PCBs (A), PBDEs (B) and PAHs (C) in soil

Fig. 5 Effects of different elution solvent volumes on the recoveries of PCBs (A), PBDEs (B) and PAHs (C) in soilThe elution solvent is n-hexane/dichloromethane (9∶1, by volume) mixture solution.

Table 2 Standard curve equations, coefficients of determination (R²), detection limits and quantification limits of 42 persistent organic pollutants (PCBs, PBDEs, PAHs)

Table 3 Spiked recoveries in soil of 42 persistent organic pollutants (PCBs, PBDEs, PAHs)

Table 4 Detection results of 42 persistent organic pollutants (PCBs, PBDEs, PAHs) in e-waste disposal site soils


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