ASE萃取-SPE净化-气相色谱/质谱法同时测定土壤中的16种多环芳烃和8种有机氯农药
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摘要
建立了加速溶剂萃取-Florisil柱净化-气相色谱/质谱法(GCMS)同时测定新鲜土壤中的16种多环芳烃和8种有机氯农药的分析方法。通过优化GCMS分析参数和ASE条件,用选择离子模式(SIM)检测。结果表明,方法在10～600μg/L范围内线性关系良好,相关系数均大于0.996,各目标化物的方法检出限为0.10～0.31μg/kg,空白硅藻土样品的加标回收率在63.1%～86.7%之间,7次平行测定的相对标准偏差为4.9%～15.1%。用该方法测定云南某地的3个土壤样品,多环芳烃和有机氯农药均有检出,其中多环芳烃质量分数在0.9×10~(-3)～4.7×10~(-3)mg/kg之间,有机氯质量分数在0.8×10~(-3)～6.6×10~(-3)mg/kg之间,适用于土壤样品中多环芳烃和有机氯农药的分析。
This study established a method for determination of 16 kinds of polycyclic aromatic hydrocarbons and 8 kinds of organochlorine pesticides in soil samples by gas chromatography/mass spectrometry with accelerated solvent extraction.The GCMS analysis parameters and accelerated solvent extraction condition were optimized so that all the target compounds were determined by GC/MS in selective ion mode(SIM).The results showed a good linear relationship with correlation coefficients greater than 0.996in range from 10 to 600μg/L.The detection limits of the compounds were from 0.10μg/kg to 0.31μg/kg.And the recoveries of blank samples diatomite were between 63.1%and 86.7%,seven paralle samples were determined and the relative standard deviations were between 4.5%and 15.1%.The Three practical soil samples from yunnan were determined by using this method,PAHs and OCPs were detected,the PAHs residues ranged from 0.9×10~(-3)mg/kg to 4.7×10~(-3)mg/kg,the OCPs residues ranged from 0.8×10~(-3)mg/kg to 6.6×10~(-3)mg/kg.The method is suitable for the determination of PAHs and OCPs in soil.
This study established a method for determination of 16 kinds of polycyclic aromatic hydrocarbons and 8 kinds of organochlorine pesticides in soil samples by gas chromatography/mass spectrometry with accelerated solvent extraction.The GCMS analysis parameters and accelerated solvent extraction condition were optimized so that all the target compounds were determined by GC/MS in selective ion mode(SIM).The results showed a good linear relationship with correlation coefficients greater than 0.996in range from 10 to 600μg/L.The detection limits of the compounds were from 0.10μg/kg to 0.31μg/kg.And the recoveries of blank samples diatomite were between 63.1%and 86.7%,seven paralle samples were determined and the relative standard deviations were between 4.5%and 15.1%.The Three practical soil samples from yunnan were determined by using this method,PAHs and OCPs were detected,the PAHs residues ranged from 0.9×10~(-3)mg/kg to 4.7×10~(-3)mg/kg,the OCPs residues ranged from 0.8×10~(-3)mg/kg to 6.6×10~(-3)mg/kg.The method is suitable for the determination of PAHs and OCPs in soil.
引文
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[7]张晓梅,张竹青,黄文鹏.超声萃取-高效液相色谱法测定土壤中多环芳烃[J].环境科学与管理,2010,35(7):124-127.
[8]郑桂媛.快速溶剂萃取-气相色谱三重四级杆串联质谱法测定土壤中六六六和滴滴涕[J].环境与可持续发展,2017,42(4):116-117.
[9]朱恒怡,柳文媛,丁曦宁,等.气相色谱-双柱双电子捕获检测器测定土壤及沉积物中23种有机氯农药[J].色谱,2011,29(8):773-780.
[10]王新成,赵金,赵汝松,等.加速溶剂提取气-质联用分析土壤中的多环芳烃[J].中国环境监测,2014,30(3):144-148.
[11]卢福峰,邢核,许秀艳,等.ASE萃取-SPE净化-HPLC法测定土壤中多环芳烃[J].环境监测管理与技术,2007,19(3):25-27.
[12]环境保护部.环境监测分析方法标准制修订技术导则:HJ 168-2010[S].北京:中国环境科学出版社,2010.
[2]姬艳梅,王小文,梁宝翠,等.土壤中有机氯农药的污染状况与生态毒性研究[J].农业灾害研究,2012,(2):41-43.
[3]杨代凤,刘腾飞,谢修庆,等.我国农业土壤中持久性有机氯类农药污染现状分析[J].环境与可持续发展,2017,42(4):40-43.
[4]葛成军,唐文浩,黄占斌,等.土壤中多环芳烃不同前处理分析方法的比较[J].农业环境科学学报,2009,28(4):859-864.
[5]李海燕,李楠,于丹丹.微波萃取-气质联用测定土壤中的16种多环芳烃[J].环境监控与预警,2010,2(1):20-23.
[6]房丽萍,邱赫男,王伟,等.土壤和沉积物中多环芳烃分析技术研究进展[J].理化检验-化学分册,2015,51(9):1339-1346.
[7]张晓梅,张竹青,黄文鹏.超声萃取-高效液相色谱法测定土壤中多环芳烃[J].环境科学与管理,2010,35(7):124-127.
[8]郑桂媛.快速溶剂萃取-气相色谱三重四级杆串联质谱法测定土壤中六六六和滴滴涕[J].环境与可持续发展,2017,42(4):116-117.
[9]朱恒怡,柳文媛,丁曦宁,等.气相色谱-双柱双电子捕获检测器测定土壤及沉积物中23种有机氯农药[J].色谱,2011,29(8):773-780.
[10]王新成,赵金,赵汝松,等.加速溶剂提取气-质联用分析土壤中的多环芳烃[J].中国环境监测,2014,30(3):144-148.
[11]卢福峰,邢核,许秀艳,等.ASE萃取-SPE净化-HPLC法测定土壤中多环芳烃[J].环境监测管理与技术,2007,19(3):25-27.
[12]环境保护部.环境监测分析方法标准制修订技术导则:HJ 168-2010[S].北京:中国环境科学出版社,2010.