GC-MS Determination of 12 PAHs in Sludge with Ultrasonic Assisted Extraction and Solid Phase Extraction
摘 要
污泥样品(约1 g)经30 mL的体积比为1∶1的乙酸乙酯和丙酮的混合液超声提取1.0 h。离心后,取上清液,用硅固相萃取柱进行净化,采用气相色谱-质谱法测定净化液中12种多环芳烃的含量。在气相色谱分离中采用HP-5MS石英毛细管色谱柱,在质谱分析中采用选择离子监测模式。12种PAHs的质量分数均在5~500 μg·kg-1内与其对应的峰面积呈线性关系,检出限为2.29~14.50 μg·kg-1。以空白污泥样品为基体进行加标回收试验,所得回收率为54.9%~108%,测定值的相对标准偏差(n=7)为0.10%~5.4%。
Abstract
The sludge sample (about 1 g) was extracted ultrasonically for 1.0 h with 30 mL of mixed solution of ethyl acetate and acetone with volume ratio of 1:1. After centrifugation, the supernatant was taken and purified with solid phase extraction column of silicon. GC-MS was applied to the determination of 12 PAHs in the purified liquid. The HP-5MS quartz capillary chromatographic column was used for GC separation and the selected ion monitoring mode was adopted in MS determination. Linear relationships between values of peak area and mass fraction of the 12 PAHs were kept in the same range of 5-500 μg·kg-1, with detection limits in the range of 2.29-14.50 μg·kg-1. On the base of blank sludge sample, test for recovery was made by standard addition method; values of recovery found were in the range of 54.9%-108%, with RSDs (n=7) of determined values in the range of 0.10%-5.4%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202002009
所属栏目 工作简报
基金项目
收稿日期 2019/10/21
修改稿日期
网络出版日期
作者单位点击查看
备注王梓,硕士研究生,研究方向为环境化学
引用该论文: WANG Zi,YANG Zhaoguang,LI Haipu. GC-MS Determination of 12 PAHs in Sludge with Ultrasonic Assisted Extraction and Solid Phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(2): 172~178
王梓,杨兆光,李海普. 超声辅助提取-固相萃取-气相色谱-质谱法测定污泥中12种多环芳烃[J]. 理化检验-化学分册, 2020, 56(2): 172~178
共有人对该论文发表了看法,其中:
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
参考文献
【1】包贞,潘志彦,杨晔,等.环境中多环芳烃的分布及降解[J].浙江工业大学学报, 2003,31(5):528-533.
【2】许丹丹,饶竹,梁汉东.气相色谱-质谱法同时测定地下水中36种多环芳烃及其衍生物[J].理化检验-化学分册, 2019,55(1):31-38.
【3】张卫东,ZOU L Y,LI Y C,等.不同木柴在两种条件下燃烧生成的颗粒物中多环芳烃的排放特性研究[J].中国环境监测, 2003,19(5):23-27.
【4】赵文昌,程金平,谢海,等.环境中多环芳烃(PAHs)的来源与监测分析方法[J].环境科学与技术, 2006,29(3):105-107.
【5】王杰,侯伟,庞香蕊,等.不同提取方法对污泥中16种多环芳烃含量测定的影响[J].辽宁大学学报(自然科学版), 2019,46(2):162-166.
【6】KESHAVARZIFARD M, ZAKARIA M P, HWAI T S, et al. Distributions and source apportionment of sediment-associated polycyclic aromatic hydrocarbons (PAHs) and hopanes in rivers and estuaries of Peninsular Malaysia[J]. Environmental Science and Pollution Research, 2015,22(12):9424-9437.
【7】黄东勤,王盛才,陈一清,等.加速溶剂萃取-高效液相色谱法测定土壤中16种多环芳烃[J].中国环境监测, 2008,24(3):26-29.
【8】邵永怡.加速溶剂萃取/气质联用法测定城市污水处理厂污泥中的多环芳烃[J].化学分析计量, 2008,17(6):70-72.
【9】VILLAR P, CALLEJÓN M, ALONSO E, et al. Optimization and validation of a new method of analysis for polycyclic aromatic hydrocarbons in sewage sludge by liquid chromatography after microwave assisted extraction[J]. Analytica Chimica Acta, 2004,524(1/2):295-304.
【10】彭驰,廖晓兰,王美娥.自动索氏-固相萃取-GC/MS测定土壤中多环芳烃方法的建立[J].湖南农业科学, 2009(6):57-60.
【11】王丽霞,张敬轩,李挥,等.自动索氏提取-高效液相色谱法同时测定油炸面制品中的16种多环芳烃[J].河北省科学院学报, 2009,26(1):43-46.
【12】冯小康,朱强.气相色谱-质谱法测定土壤中16种多环芳烃[J].安徽农业科学, 2019,47(14):220-223.
【13】徐为中,孙忠岩,吴迪,等.固体废物中多环芳烃萃取的前处理技术及测定方法综述[J].净水技术, 2015,34(2):9-13.
【14】孙红杰,赵轶男,安晓雯,等.超声萃取-GC/MS法测定污泥生态稳定化中多环芳烃[J].大连海事大学学报, 2010,36(3):116-119.
【15】陈东洋,张昊,冯家力,等.沉积物中15种多环芳烃的凝胶渗透色谱-高效液相色谱法[J].中国卫生检验杂志, 2017,27(20):2896-2899.
【16】陈金花,宋春生,张建华.乙酸乙酯加速溶剂萃取-高效液相色谱法测定土壤中的多环芳烃[J].福建分析测试, 2010,19(1):19-23.
【17】MALISZEWSKA-KORDYBACH B, KLIMKOWICZ-PAWLAS A, SMRECZAK B, et al. Ecotoxic effect of phenanthrene on nitrifying bacteria in soils of different properties[J]. Journal of Environmental Quality, 2007,36(6):1635-1645.
【2】许丹丹,饶竹,梁汉东.气相色谱-质谱法同时测定地下水中36种多环芳烃及其衍生物[J].理化检验-化学分册, 2019,55(1):31-38.
【3】张卫东,ZOU L Y,LI Y C,等.不同木柴在两种条件下燃烧生成的颗粒物中多环芳烃的排放特性研究[J].中国环境监测, 2003,19(5):23-27.
【4】赵文昌,程金平,谢海,等.环境中多环芳烃(PAHs)的来源与监测分析方法[J].环境科学与技术, 2006,29(3):105-107.
【5】王杰,侯伟,庞香蕊,等.不同提取方法对污泥中16种多环芳烃含量测定的影响[J].辽宁大学学报(自然科学版), 2019,46(2):162-166.
【6】KESHAVARZIFARD M, ZAKARIA M P, HWAI T S, et al. Distributions and source apportionment of sediment-associated polycyclic aromatic hydrocarbons (PAHs) and hopanes in rivers and estuaries of Peninsular Malaysia[J]. Environmental Science and Pollution Research, 2015,22(12):9424-9437.
【7】黄东勤,王盛才,陈一清,等.加速溶剂萃取-高效液相色谱法测定土壤中16种多环芳烃[J].中国环境监测, 2008,24(3):26-29.
【8】邵永怡.加速溶剂萃取/气质联用法测定城市污水处理厂污泥中的多环芳烃[J].化学分析计量, 2008,17(6):70-72.
【9】VILLAR P, CALLEJÓN M, ALONSO E, et al. Optimization and validation of a new method of analysis for polycyclic aromatic hydrocarbons in sewage sludge by liquid chromatography after microwave assisted extraction[J]. Analytica Chimica Acta, 2004,524(1/2):295-304.
【10】彭驰,廖晓兰,王美娥.自动索氏-固相萃取-GC/MS测定土壤中多环芳烃方法的建立[J].湖南农业科学, 2009(6):57-60.
【11】王丽霞,张敬轩,李挥,等.自动索氏提取-高效液相色谱法同时测定油炸面制品中的16种多环芳烃[J].河北省科学院学报, 2009,26(1):43-46.
【12】冯小康,朱强.气相色谱-质谱法测定土壤中16种多环芳烃[J].安徽农业科学, 2019,47(14):220-223.
【13】徐为中,孙忠岩,吴迪,等.固体废物中多环芳烃萃取的前处理技术及测定方法综述[J].净水技术, 2015,34(2):9-13.
【14】孙红杰,赵轶男,安晓雯,等.超声萃取-GC/MS法测定污泥生态稳定化中多环芳烃[J].大连海事大学学报, 2010,36(3):116-119.
【15】陈东洋,张昊,冯家力,等.沉积物中15种多环芳烃的凝胶渗透色谱-高效液相色谱法[J].中国卫生检验杂志, 2017,27(20):2896-2899.
【16】陈金花,宋春生,张建华.乙酸乙酯加速溶剂萃取-高效液相色谱法测定土壤中的多环芳烃[J].福建分析测试, 2010,19(1):19-23.
【17】MALISZEWSKA-KORDYBACH B, KLIMKOWICZ-PAWLAS A, SMRECZAK B, et al. Ecotoxic effect of phenanthrene on nitrifying bacteria in soils of different properties[J]. Journal of Environmental Quality, 2007,36(6):1635-1645.
相关信息