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

doi:10.3724/SP.J.1123.2019.12028

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

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

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 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/Abstract

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

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.

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.

图/表 7

参考文献

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Analyte	Quantitative ion (m/z)	Qualitative ions (m/z)	Retention time/min
Naphthalene	128	129	7.54
Acenaphthylene	152	151, 153	7.62
Acenaphthene	154	153, 152	7.91
Fluorene	166	165, 167	8.86
Phenanthrene	178	179, 176	11.8
Anthracene	178	179, 176	12.0
Fluoranthene	202	200, 203,	16.2
		101, 100
Pyrene	202	200, 203,	16.9
		101, 100
Benzo(a)anthracene	228	226, 229,	20.48
		114, 113
Chrysene	228	226, 229,	20.60
		114, 113
Benzo(b)fluoranthene	252	253, 250	22.98
Benzo(k)fluoranthene	252	253, 250	23.04
Benzo(a)pyrene	252	253, 250	23.70
Indeno(1, 2, 3-cd)pyrene	276	277	26.88
Dibenzo(a, h)anthracene	278	279	27.02
Benzo(g, h, i)perylene	276	274	27.74
α-HCH	183	181, 109	10.33
Hexachlorobenzene	284	286, 282	10.57
β-BHC	181	183, 109	11.15
γ-BHC	183	181, 109	11.39
δ-BHC	183	181, 109	12.29
Heptachlor	100	272, 274	13.96
Aldrin	66	263, 220	15.01
Heptachlor epoxide	353	355, 351	16.14
α-Chlordane	373	375, 377	16.75
Endosulfan Ⅰ	195	339, 341	17.06
γ-Chlordane	375	237, 272	17.13
Dieldrin	79	263, 279	17.67
p, p′-DDE	246	248, 176	17.87
Endrin	263	82, 81	18.19
EndosulfanⅡ	337	339, 341	18.40
p, p′-DDD	235	237, 165	18.62
o, p′-DDT	235	237, 165	18.68
Endrin aldehyde	67	345, 250	18.83
Endosulfan sulfate	272	387, 422	19.34
p, p′-DDT	235	237, 165	19.42
Endrin ketone	67	317, 147	20.37
Methoxychlor	227	228, 152, 274	21.41
Mirex	272	274, 270	22.86

Analyte	Quantitative ion (m/z)	Qualitative ions (m/z)	Retention time/min
Naphthalene	128	129	7.54
Acenaphthylene	152	151, 153	7.62
Acenaphthene	154	153, 152	7.91
Fluorene	166	165, 167	8.86
Phenanthrene	178	179, 176	11.8
Anthracene	178	179, 176	12.0
Fluoranthene	202	200, 203,	16.2
		101, 100
Pyrene	202	200, 203,	16.9
		101, 100
Benzo(a)anthracene	228	226, 229,	20.48
		114, 113
Chrysene	228	226, 229,	20.60
		114, 113
Benzo(b)fluoranthene	252	253, 250	22.98
Benzo(k)fluoranthene	252	253, 250	23.04
Benzo(a)pyrene	252	253, 250	23.70
Indeno(1, 2, 3-cd)pyrene	276	277	26.88
Dibenzo(a, h)anthracene	278	279	27.02
Benzo(g, h, i)perylene	276	274	27.74
α-HCH	183	181, 109	10.33
Hexachlorobenzene	284	286, 282	10.57
β-BHC	181	183, 109	11.15
γ-BHC	183	181, 109	11.39
δ-BHC	183	181, 109	12.29
Heptachlor	100	272, 274	13.96
Aldrin	66	263, 220	15.01
Heptachlor epoxide	353	355, 351	16.14
α-Chlordane	373	375, 377	16.75
Endosulfan Ⅰ	195	339, 341	17.06
γ-Chlordane	375	237, 272	17.13
Dieldrin	79	263, 279	17.67
p, p′-DDE	246	248, 176	17.87
Endrin	263	82, 81	18.19
EndosulfanⅡ	337	339, 341	18.40
p, p′-DDD	235	237, 165	18.62
o, p′-DDT	235	237, 165	18.68
Endrin aldehyde	67	345, 250	18.83
Endosulfan sulfate	272	387, 422	19.34
p, p′-DDT	235	237, 165	19.42
Endrin ketone	67	317, 147	20.37
Methoxychlor	227	228, 152, 274	21.41
Mirex	272	274, 270	22.86

Analyte	Linear regression equation	r²	LOD/(μg/kg)	LOQ/(μg/kg)	5 μg/kg		50 μg/kg		150 μg/kg
Analyte	Linear regression equation	r²	LOD/(μg/kg)	LOQ/(μg/kg)	Recovery/%	RSD/%	Recovery/%	RSD/%	Recovery/%	RSD/%
y: peak area of the target analyte; x: content of the target analyte, μg/kg.
Naphthalene	y=5.09x-8.16	1.0000	0.10	0.40	78.1	7.2	69.3	8.1	111.5	4.3
Acenaphthylene	y=9.05x-9.23	0.9998	0.04	0.16	100.3	6.0	72.9	5.3	88.7	9.8
Acenaphthene	y=6.90x-8.66	0.9998	0.04	0.16	85.5	4.4	87.2	5.5	70.7	9.8
Fluorene	y=8.36x-10.70	1.0000	0.05	0.20	93.5	2.2	72.8	3.5	104.5	6.5
Phenanthrene	y=5.53x-12.56	0.9998	0.05	0.20	76.0	5.6	83.9	6.0	92.7	6.4
Anthracene	y=4.68x-7.78	0.9999	0.11	0.44	74.1	7.0	83.2	4.1	74.9	3.9
Fluoranthene	y=4.95x-9.88	0.9998	0.10	0.40	77.0	9.7	102.2	7.0	74.2	4.6
Pyrene	y=5.22x-9.31	0.9996	0.06	0.24	88.9	7.3	90.5	8.9	80.7	10.2
Benzo(a)anthracene	y=4.87x-9.70	0.9996	0.07	0.28	83.9	14.8	93.0	3.9	100.4	8.1
Chrysene	y=5.96x-24.29	0.9992	0.08	0.32	79.0	16.8	101.2	9.0	102.6	9.2
Benzo(b)fluoranthene	y=6.21x-28.04	0.9985	0.09	0.36	103.1	26.2	98.3	6.0	63.9	8.2
Benzo(k)fluoranthene	y=7.42x-26.04	0.9989	0.12	0.48	102.6	16.3	98.1	4.1	73.4	2.4
Benzo(a)pyrene	y=5.59x-22.39	0.9991	0.04	0.16	82.9	20.8	96.3	7.0	73.8	3.4
Indeno(1, 2, 3-cd)pyrene	y=3.65x-17.01	0.9996	0.04	0.16	92.3	6.9	95.3	8.9	88.1	3.5
Dibenzo(a, h)anthracene	y=3.63x-4.29	0.9988	0.08	0.32	72.6	20.4	101.1	3.9	92.2	3.9
Benzo(g, h, i)perylene	y=5.32x-21.39	0.9991	0.05	0.20	106.3	1.4	93.8	9.0	93.8	7.8
α-HCH	y=5.00x-13.25	0.9999	0.90	3.60	80.8	2.5	84.3	13.1	80.9	2.9
Hexachlorobenzene	y=6.58x-17.14	0.9996	0.40	1.61	76.9	0.4	80.5	12.6	93.2	1.9
β-BHC	y=3.78x-12.09	0.9996	0.40	1.61	70.4	0.8	78.9	2.9	99.7	9.2
γ-BHC	y=4.24x-12.67	0.9996	0.50	2.01	91.4	2.5	90.2	2.3	109.3	19.2
δ-BHC	y=3.79x-10.76	0.9996	0.50	2.01	92.5	5.5	82.4	2.6	103.6	17.5
Heptachlor	y=2.96x-10.82	0.9996	1.16	4.64	100.4	6.4	89.2	7.0	101.8	7.1
Aldrin	y=2.85x-3.15	0.9998	0.89	3.56	80.8	12.3	77.2	9.7	110.4	6.6
Heptachlor epoxide	y=1.24x-3.56	0.9995	0.60	2.42	105.1	15.7	68.9	7.3	99.4	5.6
α-Chlordane	y=1.73x-7.36	0.9991	0.70	2.82	74.8	14.6	69.0	14.8	82.8	10.1
Endosulfan Ⅰ	y=0.85x-1.88	0.9998	0.81	3.22	83.4	13.8	90.4	3.9	86.2	10.6
γ-Chlordane	y=1.49x-5.17	0.9991	0.91	3.62	103.1	13.7	67.2	9.0	89.8	12.3
Dieldrin	y=4.39x-7.49	0.9994	1.21	4.83	102.0	12.5	80.6	6.0	86.4	1.6
p, p′-DDE	y=7.29x-20.85	0.9998	0.40	1.61	80.3	2.2	87.5	4.1	77.2	7.6
Endrin	y=0.66x-1.48	0.9997	0.96	3.84	102.9	12.6	83.6	15.7	78.0	6.9
EndosulfanⅡ	y=0.83x-0.64	0.9995	0.85	3.40	84.0	4.0	78.8	14.6	88.5	9.3
p, p′-DDD	y=8.00x-8.52	0.9999	0.88	3.52	101.2	4.4	77.5	13.8	70.9	6.0
p, p′-DDT	y=6.23x-32.06	0.9994	1.05	4.20	98.8	2.2	100.3	16.3	90.5	5.6
Endrin aldehyde	y=0.39x-1.42	0.9997	0.76	3.04	78.1	0.6	90.5	20.8	87.6	11.1
Endosulfan sulfate	y=1.00x-2.11	0.9998	0.85	3.40	70.9	1.0	98.2	6.9	76.6	9.2
p, p′-DDT	y=5.39x-23.81	0.9994	0.78	3.12	90.2	0.8	86.2	20.4	75.0	2.8
Endrin ketone	y=1.03x-2.22	0.9991	0.65	2.60	87.6	1.0	87.2	1.4	74.6	3.9
Methoxychlor	y=10.49x-52.53	0.9992	0.55	2.20	85.1	0.8	88.9	10.5	86.4	3.3
Mirex	y=4.25x-13.66	0.9997	1.00	4.00	90.3	1.0	112.1	9.9	75.6	6.4

Analyte	Linear regression equation	r²	LOD/(μg/kg)	LOQ/(μg/kg)	5 μg/kg		50 μg/kg		150 μg/kg
Analyte	Linear regression equation	r²	LOD/(μg/kg)	LOQ/(μg/kg)	Recovery/%	RSD/%	Recovery/%	RSD/%	Recovery/%	RSD/%
y: peak area of the target analyte; x: content of the target analyte, μg/kg.
Naphthalene	y=5.09x-8.16	1.0000	0.10	0.40	78.1	7.2	69.3	8.1	111.5	4.3
Acenaphthylene	y=9.05x-9.23	0.9998	0.04	0.16	100.3	6.0	72.9	5.3	88.7	9.8
Acenaphthene	y=6.90x-8.66	0.9998	0.04	0.16	85.5	4.4	87.2	5.5	70.7	9.8
Fluorene	y=8.36x-10.70	1.0000	0.05	0.20	93.5	2.2	72.8	3.5	104.5	6.5
Phenanthrene	y=5.53x-12.56	0.9998	0.05	0.20	76.0	5.6	83.9	6.0	92.7	6.4
Anthracene	y=4.68x-7.78	0.9999	0.11	0.44	74.1	7.0	83.2	4.1	74.9	3.9
Fluoranthene	y=4.95x-9.88	0.9998	0.10	0.40	77.0	9.7	102.2	7.0	74.2	4.6
Pyrene	y=5.22x-9.31	0.9996	0.06	0.24	88.9	7.3	90.5	8.9	80.7	10.2
Benzo(a)anthracene	y=4.87x-9.70	0.9996	0.07	0.28	83.9	14.8	93.0	3.9	100.4	8.1
Chrysene	y=5.96x-24.29	0.9992	0.08	0.32	79.0	16.8	101.2	9.0	102.6	9.2
Benzo(b)fluoranthene	y=6.21x-28.04	0.9985	0.09	0.36	103.1	26.2	98.3	6.0	63.9	8.2
Benzo(k)fluoranthene	y=7.42x-26.04	0.9989	0.12	0.48	102.6	16.3	98.1	4.1	73.4	2.4
Benzo(a)pyrene	y=5.59x-22.39	0.9991	0.04	0.16	82.9	20.8	96.3	7.0	73.8	3.4
Indeno(1, 2, 3-cd)pyrene	y=3.65x-17.01	0.9996	0.04	0.16	92.3	6.9	95.3	8.9	88.1	3.5
Dibenzo(a, h)anthracene	y=3.63x-4.29	0.9988	0.08	0.32	72.6	20.4	101.1	3.9	92.2	3.9
Benzo(g, h, i)perylene	y=5.32x-21.39	0.9991	0.05	0.20	106.3	1.4	93.8	9.0	93.8	7.8
α-HCH	y=5.00x-13.25	0.9999	0.90	3.60	80.8	2.5	84.3	13.1	80.9	2.9
Hexachlorobenzene	y=6.58x-17.14	0.9996	0.40	1.61	76.9	0.4	80.5	12.6	93.2	1.9
β-BHC	y=3.78x-12.09	0.9996	0.40	1.61	70.4	0.8	78.9	2.9	99.7	9.2
γ-BHC	y=4.24x-12.67	0.9996	0.50	2.01	91.4	2.5	90.2	2.3	109.3	19.2
δ-BHC	y=3.79x-10.76	0.9996	0.50	2.01	92.5	5.5	82.4	2.6	103.6	17.5
Heptachlor	y=2.96x-10.82	0.9996	1.16	4.64	100.4	6.4	89.2	7.0	101.8	7.1
Aldrin	y=2.85x-3.15	0.9998	0.89	3.56	80.8	12.3	77.2	9.7	110.4	6.6
Heptachlor epoxide	y=1.24x-3.56	0.9995	0.60	2.42	105.1	15.7	68.9	7.3	99.4	5.6
α-Chlordane	y=1.73x-7.36	0.9991	0.70	2.82	74.8	14.6	69.0	14.8	82.8	10.1
Endosulfan Ⅰ	y=0.85x-1.88	0.9998	0.81	3.22	83.4	13.8	90.4	3.9	86.2	10.6
γ-Chlordane	y=1.49x-5.17	0.9991	0.91	3.62	103.1	13.7	67.2	9.0	89.8	12.3
Dieldrin	y=4.39x-7.49	0.9994	1.21	4.83	102.0	12.5	80.6	6.0	86.4	1.6
p, p′-DDE	y=7.29x-20.85	0.9998	0.40	1.61	80.3	2.2	87.5	4.1	77.2	7.6
Endrin	y=0.66x-1.48	0.9997	0.96	3.84	102.9	12.6	83.6	15.7	78.0	6.9
EndosulfanⅡ	y=0.83x-0.64	0.9995	0.85	3.40	84.0	4.0	78.8	14.6	88.5	9.3
p, p′-DDD	y=8.00x-8.52	0.9999	0.88	3.52	101.2	4.4	77.5	13.8	70.9	6.0
p, p′-DDT	y=6.23x-32.06	0.9994	1.05	4.20	98.8	2.2	100.3	16.3	90.5	5.6
Endrin aldehyde	y=0.39x-1.42	0.9997	0.76	3.04	78.1	0.6	90.5	20.8	87.6	11.1
Endosulfan sulfate	y=1.00x-2.11	0.9998	0.85	3.40	70.9	1.0	98.2	6.9	76.6	9.2
p, p′-DDT	y=5.39x-23.81	0.9994	0.78	3.12	90.2	0.8	86.2	20.4	75.0	2.8
Endrin ketone	y=1.03x-2.22	0.9991	0.65	2.60	87.6	1.0	87.2	1.4	74.6	3.9
Methoxychlor	y=10.49x-52.53	0.9992	0.55	2.20	85.1	0.8	88.9	10.5	86.4	3.3
Mirex	y=4.25x-13.66	0.9997	1.00	4.00	90.3	1.0	112.1	9.9	75.6	6.4

Analyte	Sample 1	Sample 2	Sample 3
-: not detected or detected value below LOQ.
Naphthalene	12.2	22.6	16.2
Acenaphthylene	-	87.2	9.8
Acenaphthene	21.6	67.6	-
Fluorene	4.6	89.1	12.6
Phenanthrene	15.6	-	18.9
Anthracene	18.1	19.8	-
Fluoranthene	16.2	22.2	23.5
Pyrene	5.2	-	5.8
Benzo(a)anthracene	-	36.6	-
Chrysene	6.6	65.6	8.1
Benzo(b)fluoranthene	10.1	62.2	-
Benzo(k)fluoranthene	8.2	3.8	78.2
Benzo(a)pyrene	5.8	19.6	3.8
Indeno(1, 2, 3-cd)pyrene	11.2	26.8	5.3
Dibenzo(a, h)anthracene	9.3	18.9	1.2
Benzo(g, h, i)perylene	20.6	20.6	-
α-HCH	-	-	15.6
Hexachlorobenzene	10.6	32.1	28.8

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

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

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