GC Determination of 15 Organchlorine Pesticides and Polychlorobiphenyls in Soil
摘 要
应用气相色谱法测定土壤中15种有机氯农药(OCP′s)及多氯联苯(PCB′s)。土壤样品(10 g)用正己烷-丙酮(1+1)混合液160 mL在65 ℃水浴中索氏提取4 h,所得提取液用硫酸分次进行磺化净化。净化后的溶液氮吹浓缩至0.5 mL,用正己烷定容至1 mL。分取1 μL进样,用HP-1色谱柱分离,用电子捕获检测器(ECD)检测。所测15种OCP′s和PCB′s的质量浓度均在1.0~100 μg·L-1范围内与其峰面积呈线性关系,15种化合物的检出限(3S/N)在0.080~0.16 ng·g-1之间。在空白样品中加入15种化合物的混合标准溶液10.0 ng进行回收试验,测得回收率在86.4%~108%之间,其测定值的相对标准偏差(n=7)在2.4%~5.2%之间。
Abstract
GC was applied to the determination of 15 organochlorine pesticides (OCP′s) and polychlorobiphenyls (PCB′s) in soil. The soil sample (10 g) was extracted with 160 mL of a mixture of n-hexane and acetone (1+1) in a water bath at 65 ℃ by soxhlet extraction for 4 h. The extract was then purified by sulfonation through shaking with portions of H2SO4. The solution was concentrated to ca. 0.5 mL by N2-blowing and made up to 1 mL with n-hexane. An aliquot of 1 μL was introduced into the HP-1 column for GC separation. ECD was used in detection. Linear relationships between values of peak area and mass concentration of the 15 compounds were kept in the same range of 1.0-100 μg·L-1, with their detection limits (3S/N) in the range of 0.080-0.16 ng·g-1. Recovery was tested by adding 20 ng of mixed standard solution of the 15 compounds to a blank sample as matrix, giving values of recovery in the range from 86.4% to 108%, with RSD′s (n=7) ranged from 2.4% to 5.2%.
中图分类号 O657.31
所属栏目 工作简报
基金项目
收稿日期 2013/9/27
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备注郝原芳(1965-),女,辽宁沈阳人,高级工程师,主要从事地下水污染调查。
引用该论文: HAO Yuan-fang,LI Li-jun,MA Jian-sheng,WANG Hai-jiao,WANG Xin. GC Determination of 15 Organchlorine Pesticides and Polychlorobiphenyls in Soil[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2014, 50(10): 1228~1231
郝原芳,李丽君,马健生,王海娇,王鑫. 气相色谱法测定土壤中15种有机氯和多氯联苯[J]. 理化检验-化学分册, 2014, 50(10): 1228~1231
被引情况:
【1】施婷婷,司雄元,檀华蓉,司友斌,刘 伟, "联苯类分子印迹聚合物在气相色谱法测定联苯及3,3-二氯联苯中的应用",理化检验-化学分册 52, 869-873(2016)
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参考文献
【1】GB 13015-1991含多氯联苯废物污染控制标准 附录A 废物中多氯联苯(PCB)的测定[S].
【2】EPA 8270cSemivolatile organic compoundsby gas chromatography/mass spectrometry (GC/MS)[S].
【3】EPA 8082Polychlorinated biphenyls (PCBs) by gas chromatography[S].
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【10】任曼,彭平安,张素坤,等.气相色谱/高分辨质谱联用测定环境样品中的二噁英和类二噁英多氯联苯[J].分析化学, 2007,35(2): 176-180.
【11】谢振伟,杨坪,廖翀,等.串联四极杆质谱(GC-QqQ-MS/MS)测定土壤中的有机氯农药和多氯联苯[J].中国环境监测, 2008,24(5): 20-24.
【12】邓安平.酶联免疫吸附分析法测定苯并(a)芘和多氯联苯[J].环境化学, 2006,25(3): 340-343.
【13】李国刚,李红莉.持久性有机污染物在中国的环境监测现状[J].中国环境监测, 2004,20(4): 5360-5360.
【14】申中兰,蔡继宝,高芸.基质固相分散-加速溶剂萃取-气相色谱法测定土壤中有机氯农药残留[J].分析化学, 2005,33(9): 1318-1320.
【15】佟玲,黄园英,张玲金,等.土壤中持久性有机污染物分析的前处理方法[J].岩矿测试, 2008,27(2): 81-86.
【16】黄园英,佟玲,张玲金,等.用ASE提取和GPC净化气相色谱法快速测定土壤中痕量有机氯代化合物[J].生态环境, 2008,17(1): 184-189.
【17】江奎,汪雨,支辛辛,等.加速溶剂萃取/GC-ECD分析土壤中多氯联苯的研究[J].青岛大学学报, 2006,21(1): 18-22.
【18】FROST S P, DEAN J R, EVANS K P, et al. Extraction of hexaconazole fromweathered soils: a comparison between soxhletextraction, microwave-assited extraction, supercriticalfluid extraction and accelerated solvent extraction[J]. Analyst, 1997,122: 895-898.
【19】LI K, LANDRIAULT M, FINGAS M, et al. Acceleratedsolvent extraction (ASE) of environmental organiccompounds in soils using a modified supercritical fluidextractor[J]. Journal of Hazardous Materials, 2003,102: 93-104.
【20】WANG W T, MENG B J, LU X X, et al. Extraction of polycyclic aromatic hydrocarbons andorganochlorine pesticides from soils: a comparisonbetween soxhlet extraction, microwave-assistedextraction and accelerated solvent extraction technique[J]. Analytica Chimica Acta, 2007,602: 211-222.
【21】谢湘云,沈爱斯,叶红雷.固相萃取小柱净化-气相色谱法测定土壤和沉积物中有机氯和拟除虫菊酯农药残留[J].环境化学, 2006,25(3): 347-350.
【22】朱雪梅,崔艳丽,郭丽青.用加速溶剂提取仪提取污染土壤中的有机氯农药[J].环境科学, 2002,23(5): 113-116.
【23】ABRHA Y, RAGHAVAN D. Polychlorinated biphenyl (PCB) recovery from spiked organic matrix using acceleratedsolvent extraction (ASE) and soxhlet extraction[J]. Journal of Hazardous Materials, 2000(B80): 147-157.
【24】安琼,董元华,倪俊.气相色谱法测定禽蛋中微量有机氯农药及多氯联苯的残留[J].色谱, 2002,20(2): 167-171.
【2】EPA 8270cSemivolatile organic compoundsby gas chromatography/mass spectrometry (GC/MS)[S].
【3】EPA 8082Polychlorinated biphenyls (PCBs) by gas chromatography[S].
【4】何小青,李攻科,熊国华,等.微波碱解法消除土壤样品多氯联苯测定中有机氯农药的干扰[J].分析化学, 2000,28(1): 26-30.
【5】李娟,高丹.超声波萃取-GC/MS法测定土壤中多氯联苯[J].环境监测管理与技术, 2007,19(6): 31-32.
【6】崔兆杰,赵士燕.超临界CO2流体萃取-气相色谱法测定土壤中的类二噁英类多氯联苯[J].山东大学学报: 理学版, 2006,41(6): 124-128.
【7】安琼,董元华,倪俊,等.气相色谱法测定禽蛋中微量有机氯农药及多氯联苯的残留[J].色谱,2002,20(2): 167-171.
【8】刘雯,李娟.微波萃取-双ECD气相色谱法测定土壤中的多氯联苯[J].中国环境监测, 2007,23(2): 11-16.
【9】黄业茹,施钧慧,唐莉.GC/MS分析环境样品中的多氯联苯(PCB′s)[J].分析测试技术与仪器, 2000,6(4): 216-224.
【10】任曼,彭平安,张素坤,等.气相色谱/高分辨质谱联用测定环境样品中的二噁英和类二噁英多氯联苯[J].分析化学, 2007,35(2): 176-180.
【11】谢振伟,杨坪,廖翀,等.串联四极杆质谱(GC-QqQ-MS/MS)测定土壤中的有机氯农药和多氯联苯[J].中国环境监测, 2008,24(5): 20-24.
【12】邓安平.酶联免疫吸附分析法测定苯并(a)芘和多氯联苯[J].环境化学, 2006,25(3): 340-343.
【13】李国刚,李红莉.持久性有机污染物在中国的环境监测现状[J].中国环境监测, 2004,20(4): 5360-5360.
【14】申中兰,蔡继宝,高芸.基质固相分散-加速溶剂萃取-气相色谱法测定土壤中有机氯农药残留[J].分析化学, 2005,33(9): 1318-1320.
【15】佟玲,黄园英,张玲金,等.土壤中持久性有机污染物分析的前处理方法[J].岩矿测试, 2008,27(2): 81-86.
【16】黄园英,佟玲,张玲金,等.用ASE提取和GPC净化气相色谱法快速测定土壤中痕量有机氯代化合物[J].生态环境, 2008,17(1): 184-189.
【17】江奎,汪雨,支辛辛,等.加速溶剂萃取/GC-ECD分析土壤中多氯联苯的研究[J].青岛大学学报, 2006,21(1): 18-22.
【18】FROST S P, DEAN J R, EVANS K P, et al. Extraction of hexaconazole fromweathered soils: a comparison between soxhletextraction, microwave-assited extraction, supercriticalfluid extraction and accelerated solvent extraction[J]. Analyst, 1997,122: 895-898.
【19】LI K, LANDRIAULT M, FINGAS M, et al. Acceleratedsolvent extraction (ASE) of environmental organiccompounds in soils using a modified supercritical fluidextractor[J]. Journal of Hazardous Materials, 2003,102: 93-104.
【20】WANG W T, MENG B J, LU X X, et al. Extraction of polycyclic aromatic hydrocarbons andorganochlorine pesticides from soils: a comparisonbetween soxhlet extraction, microwave-assistedextraction and accelerated solvent extraction technique[J]. Analytica Chimica Acta, 2007,602: 211-222.
【21】谢湘云,沈爱斯,叶红雷.固相萃取小柱净化-气相色谱法测定土壤和沉积物中有机氯和拟除虫菊酯农药残留[J].环境化学, 2006,25(3): 347-350.
【22】朱雪梅,崔艳丽,郭丽青.用加速溶剂提取仪提取污染土壤中的有机氯农药[J].环境科学, 2002,23(5): 113-116.
【23】ABRHA Y, RAGHAVAN D. Polychlorinated biphenyl (PCB) recovery from spiked organic matrix using acceleratedsolvent extraction (ASE) and soxhlet extraction[J]. Journal of Hazardous Materials, 2000(B80): 147-157.
【24】安琼,董元华,倪俊.气相色谱法测定禽蛋中微量有机氯农药及多氯联苯的残留[J].色谱, 2002,20(2): 167-171.
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