高级搜索

水体和甘蓝及土壤中毒死蜱残留检测方法

,  ,  , 

downloadPDF

上一篇

下一篇

谢慧, 朱鲁生, 王军, 王金花. 水体和甘蓝及土壤中毒死蜱残留检测方法[J]. 环境化学, 2012, 31(8): 1268-1274.
引用本文: 谢慧, 朱鲁生, 王军, 王金花. 水体和甘蓝及土壤中毒死蜱残留检测方法[J]. 环境化学, 2012, 31(8): 1268-1274.
shu
XIE Hui, ZHU Lusheng, WANG Jun, WANG Jinhua. Determination of chlorpyrifos residues in water, cabbage and soil by GC-FPD[J]. Environmental Chemistry, 2012, 31(8): 1268-1274.
Citation: XIE Hui, ZHU Lusheng, WANG Jun, WANG Jinhua. Determination of chlorpyrifos residues in water, cabbage and soil by GC-FPD[J]. Environmental Chemistry, 2012, 31(8): 1268-1274.
shu

水体和甘蓝及土壤中毒死蜱残留检测方法

  • 1.

    山东农业大学资源与环境学院, 泰安, 271018;

  • 2.

    山东农业大学, 山东省高校农业环境重点实验室, 泰安, 271018

  • 基金项目:

    国家自然科学基金资助项目(41071164, 40801203和 41001152)

    科技部农转资金项目(2006GB2C600168)

    山东省自主创新重大专项(2009ZHZX1B0801)

    高等学校博士学科点专项科研基金(20113702110007)资助.

Determination of chlorpyrifos residues in water, cabbage and soil by GC-FPD

  • 1.

    College of Resources and Environment, Shandong Agricultural University, Taian, 271018, China;

  • 2.

    Shandong Agricultural University, Key Laboratory of Agricultural Environment in Universities of Shandong, Taian, 271018, China

  • Fund Project:

  • 摘要: 研究运用不同的样品前处理方式,在装配火焰光度检测器的气相色谱(GC-FPD)上检测,建立了有机磷杀虫剂毒死蜱在水样、土壤和甘蓝中的残留测定方法.研究表明,不同样品中的毒死蜱残留采用本文中介绍的前处理方法是可行的,用石油醚盐析提取和净化水样中毒死蜱,采用丙酮振荡提取甘蓝中毒死蜱,选用索氏提取法提取土壤中毒死蜱,并经液液分配净化后,采用OV-101大口径毛细管柱(30 m×0.53 mm×1.0 μm),在装配火焰光度检测器(FPD和磷滤光片)的气相色谱上测定.该分析方法下,毒死蜱的保留时间为1.74 min,线性范围在1.0×10-11-1.0×10-8 g之间,其线性相关系数为0.9998,最小检出量为2.0×10-12 g.在设定的较低添加浓度的条件下,毒死蜱在水样、土壤与甘蓝上的添加回收率为80%-120%,变异系数均小于5%.该分析方法灵敏、准确、操作简便,适合水样、甘蓝和土壤中低浓度毒死蜱的残留检测.
    Abstract: Using gas chromatography-flame photometric detection (GC-FPD), a method was developed for the analysis of organophosphorus pesticide chlorpyrifos in water, soil and cabbage. The chlorpyrifos residue in water was extracted and purified by petroleum ether and liquid-liquid extraction. The chlorpyrifos residue in cabbage was extracted with acetone and the chlorpyrifos residue in soil was extracted by the Soxhlet method with acetone. After clean up by liquid-liquid distribution, it was determinated by GC-FPD equipped with OV-101 (100% dimethyl polysiloxane) column (30 m×0.53 mm×1.0 μm). The retention time of chlorpyrifos was 1.74 min; the linearity range of chlorpyrifos was between 1.0×10-11 and 1.0×10-8 g; the correlation coefficient was 0.9998; the limits of detection was 2.0×10-12 g. Average recovery rates of chlorpyrifos in these samples ranged from 80% to 120% with coefficient of variation from 1.19% to 4.40%. The method is sensitive and operated easily to detect low levels of chlorpyrifos in the water, cabbage and soil.
  • 加载中
  • [1] David S, Stuart H, Kevin R. Analytical chemistry of chlorpyrifos and diuron in aquatic ecosystems [J]. Anal Chim Acta, 1998, 360:1-16
    [2] 我国毒死蜱市场有望大幅增长[J]. 农药,2009,12:901
    [3] Schardein J L, Scialli A R. The legislation of toxicologyic safety factors: the food quality protection act with chlorpyrifos as a test case Reproductive [J]. Toxicol, 1999, 13, (1):1-14
    [4] Jia C H, Zhu X D, Zhao E C, et al. Application of SPME based on a stainless steel wire for the determination of pyrethroid insecticide residues in water and soil [J]. chromatog, 2010, 72:1219-1223
    [5] Keller J M, Swarthout R F, Carlson B K R, et al. Comparison of five extraction methods for measuring PCBs, PBDEs, organochlorine pesticides, and lipid content in serum[J]. Anal Bioanal Chem, 2009, 393: 747-760
    [6] Zhang Y P, Yang J, Shi R H, et al. Development of an analytical method based on accelerated solvent extraction, solid-phase extraction clean-up, then GC-ECD for analysis of fourteen organochlorine pesticides in cereal crops[J]. Chromatog, 2011, 73:385-391
    [7]
    [8] Syed Shahid A, Riaz U H, Mubasshirah K, et al. Use of ultra-violet spectrophotometry for determination of insecticides and aromatic hydrocarbon pollutants [J]. Punjab University J Zoology, 1997, 12: 31-34
    [9] 何奕,王琦琛,虞骥. 快速检测毒死蜱残留量的酶膜生物传感器研究[J]. 上海环境科学,2003,22 (10):687-689
    [10] 韩畅,朱鲁生,王军,等. HPLC测定水体中毒死蜱及其有毒降解产物TCP [J]. 农业环境科学学报2009,28(7):1552-1556
    [11] 张超,杨红. 水、土壤和蔬菜中毒死蜱、甲基毒死蜱残留检测前处理方法 [J]. 农药,2010,49(5):367-370
    [12] Zhang Q M, Zhu L S, Han C, et al. Analysis of chlorpyrifos and TCP residues in agricultural soil and apples by HPLC [J]. J Food Agricul & Environ, 2011, 9(1):659-662
    [13]
    [14]
    [15] 赵丽娟,张洪,秦曙,等. 毒死蜱在梨和土壤中的残留研究[J] 农药科学与管理,2010,31(2):42-46
    [16]
    [17] 黄碧燕,韦宇宁,李小夏,等. 气相色谱法同时测定土壤中毒死蜱、乙草胺和丁草胺残留量[J]. 广西科学院学报,2010,26(3):255-257
    [18] Richardson D D, Caruso J A. Screening organophosphorus nerve agent degradation products in pesticide mixtures by GC-ICPMS [J]. Anal Bioanal Chem, 2007, 389:679-682
    [19] Mukherjee I, Singh S, Sharma P K. Extraction of multi-class pesticide residues in mango fruits (Mangiferae indica L.): Application of pesticide residues in monitoring of mangoes [J]. Bull Environ Contam Toxicol, 2007, 78:380-383
    [20] Mukherjee I. Determination of pesticide residues in honey samples [J]. Bull Environ Contam Toxicol, 2009, 83:818-821
    [21] Wang S L, Yang S P, Ren L P, et al. Determination of organophosphorus pesticides in leeks (Allium porrum L.) by GC-FPD [J]. Chromatog, 2009, 69:79-84
    [22] Bishnu A, Chakrabarti K, Chakraborty A, et al. Pesticide residue level in tea ecosystems of Hill and Dooars regions of West Bengal, India [J]. Environ Monit Assess, 2009, 149:457-464
    [23] Gao Q, Hua R M, Tang F, et al. A multiresidue method for 20 pesticides in Radix paeoniae Alba of Chinese Herb by gas chromatography with electron-capture detection [J]. Bull Environ Contam Toxicol, 2010, 84:779-783
    [24] Lu J L D P. Multipesticide residue assessment of agricultural soil and water in major farming areas in Benguet, Philippines[J]. Arch Environ Contam Toxicol, 2010, 59:175-181
    [25] 孙晶.农药对水质的影响[J]. 农药译丛,1996,18(1):55-57
  • 加载中
WeChat 点击查看大图
计量
  • 文章访问数:  989
  • HTML全文浏览数:  886
  • PDF下载数:  377
  • 施引文献:  0
出版历程
  • 收稿日期:  2011-10-12
谢慧, 朱鲁生, 王军, 王金花. 水体和甘蓝及土壤中毒死蜱残留检测方法[J]. 环境化学, 2012, 31(8): 1268-1274.
引用本文: 谢慧, 朱鲁生, 王军, 王金花. 水体和甘蓝及土壤中毒死蜱残留检测方法[J]. 环境化学, 2012, 31(8): 1268-1274.
shu
XIE Hui, ZHU Lusheng, WANG Jun, WANG Jinhua. Determination of chlorpyrifos residues in water, cabbage and soil by GC-FPD[J]. Environmental Chemistry, 2012, 31(8): 1268-1274.
Citation: XIE Hui, ZHU Lusheng, WANG Jun, WANG Jinhua. Determination of chlorpyrifos residues in water, cabbage and soil by GC-FPD[J]. Environmental Chemistry, 2012, 31(8): 1268-1274.
shu

水体和甘蓝及土壤中毒死蜱残留检测方法

  • 1.  山东农业大学资源与环境学院, 泰安, 271018;
  • 2.  山东农业大学, 山东省高校农业环境重点实验室, 泰安, 271018
  • 收稿日期:  2011-10-12
基金项目:

国家自然科学基金资助项目(41071164, 40801203和 41001152)

科技部农转资金项目(2006GB2C600168)

山东省自主创新重大专项(2009ZHZX1B0801)

高等学校博士学科点专项科研基金(20113702110007)资助.

摘要: 研究运用不同的样品前处理方式,在装配火焰光度检测器的气相色谱(GC-FPD)上检测,建立了有机磷杀虫剂毒死蜱在水样、土壤和甘蓝中的残留测定方法.研究表明,不同样品中的毒死蜱残留采用本文中介绍的前处理方法是可行的,用石油醚盐析提取和净化水样中毒死蜱,采用丙酮振荡提取甘蓝中毒死蜱,选用索氏提取法提取土壤中毒死蜱,并经液液分配净化后,采用OV-101大口径毛细管柱(30 m×0.53 mm×1.0 μm),在装配火焰光度检测器(FPD和磷滤光片)的气相色谱上测定.该分析方法下,毒死蜱的保留时间为1.74 min,线性范围在1.0×10-11-1.0×10-8 g之间,其线性相关系数为0.9998,最小检出量为2.0×10-12 g.在设定的较低添加浓度的条件下,毒死蜱在水样、土壤与甘蓝上的添加回收率为80%-120%,变异系数均小于5%.该分析方法灵敏、准确、操作简便,适合水样、甘蓝和土壤中低浓度毒死蜱的残留检测.

English Abstract

    全文HTML

参考文献 (25)

返回顶部

目录

/

返回文章
返回

Copyright © 2019 中国科学院生态环境研究中心