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有机氯农药残留检测的快速样品前处理效果研究

曾艳 李霞雪 王任佑

曾艳, 李霞雪, 王任佑. 有机氯农药残留检测的快速样品前处理效果研究[J]. 分析测试技术与仪器, 2016, 22(3): 152-158. doi: 10.16495/j.1006-3757.2016.03.005
引用本文: 曾艳, 李霞雪, 王任佑. 有机氯农药残留检测的快速样品前处理效果研究[J]. 分析测试技术与仪器, 2016, 22(3): 152-158. doi: 10.16495/j.1006-3757.2016.03.005
ZENG Yan, LI Xia-xue, WANG Ren-you. Effect of QuEChERS Pretreatment on Organochlorine Pesticide Residue Detection[J]. Analysis and Testing Technology and Instruments, 2016, 22(3): 152-158. doi: 10.16495/j.1006-3757.2016.03.005
Citation: ZENG Yan, LI Xia-xue, WANG Ren-you. Effect of QuEChERS Pretreatment on Organochlorine Pesticide Residue Detection[J]. Analysis and Testing Technology and Instruments, 2016, 22(3): 152-158. doi: 10.16495/j.1006-3757.2016.03.005

有机氯农药残留检测的快速样品前处理效果研究

doi: 10.16495/j.1006-3757.2016.03.005
基金项目: 

四川省2014年农产品质量安全例行抽检项目资助 川农业函[2014]16号

详细信息
    作者简介:

    曾艳(1983-), 女, 硕士研究生, 农艺师, 主要研究方向为农产品及产地环境农药残留检测, E-mail:276874503@qq.com

  • 中图分类号: O657.3

Effect of QuEChERS Pretreatment on Organochlorine Pesticide Residue Detection

  • 摘要: 应用快速样品前处理技术(QuEChERS)与《NY/T 761-2008蔬菜和水果中有机磷、有机氯、拟除虫菊酯和氨基甲酸酯类农药多残留的测定法》(NY/T 761-2008)的前处理方法处理农产品样本,采用气相色谱检测多种农产品中有机氯农药残留量.分析了QuEChERS法前处理用于有机氯农残检测的效果.结果表明:QuEChERS法前处理测定18种有机氯农药残留加标回收率在72.1%~123.9%之间,RSD在0.5%~19.1%之间,有72.2%的农药检出限大于等于NY/T 761-2008方法,只有27.8%略低于NY/T 761-2008方法,对多种蔬菜水果的测试均符合多农残检测方法要求,结果准确可靠. QuEChERS法前处理消耗的有机溶剂少、处理速度快、选择性强、回收率高、精密度高、实用性强、安全性更高.检测有机氯农残时,可在一般情况下替代NY/T 761-2008的前处理方法.
  • 图  1  莴苣样品添加0.08 mg/Kg I组混合农药色谱图(a)Q法前处理, (b)N法前处理

    (1)666,(2)百菌清,(3)乙烯菌核利,(4)三唑酮,(5)腐霉利,(6)异菌脲,(7)甲氰菊酯,(8)三氟氯氰菊酯,(9)氟氯氰菊酯,(10)氟氰戊菊酯,(11)氟胺氰菊酯,(12)溴氰菊酯

    Figure  1.  Chromatograms of lettuce with 0.08 mg/Kg group I mixed pesticides (a) with QuEChERS pretreatment, (b) with NY/T 761-2008 pretreatment

    图  2  Q法处理多样本农药添加回收率质量控制图

    Figure  2.  Quality control chart of spiked recoveries of multi-sample pesticides by QuEChERS pretreatment

    表  1  前处理消耗对比

    Table  1.   Comparison of pretreatment consumption

    项目NY/T 761-2008QuEChERS
    样本用量25.0 g15.0 g
    乙腈用量50 mL35 mL
    正己烷用量25.5 mL2.0 mL
    丙酮用量约5 mL
    氯化钠5~7 g
    废液量(以液态计)22.0 mL2.0 mL
    单样本平均处理时间约100 min约35 min
    器皿消耗多(如刻度具塞试管、漏斗、比色管、锥形瓶等)少(只用离心管和少量具塞试管)
    下载: 导出CSV

    表  2  Q法检测各农药的检出限

    Table  2.   Detection limits (LODs) of pesticides by Q method

    农药名称检出限农药名称检出限农药名称检出限
    Q法N法Q法N法Q法N法
    6660.000 10.000 4甲氰菊酯0.0020.002三氯杀螨醇0.000 60.000 8
    百菌清0.000 10.000 3三氟氯氰菊酯0.0020.002滴滴涕0.000 50.000 3
    乙烯菌核利0.000 10.000 4氟氯氰菊酯0.0020.002联苯菊酯0.000 20.000 6
    三唑酮0.000 10.001氟氰戊菊酯0.0030.001氯菊酯0.000 10.001
    腐霉利0.0010.002氟胺氰菊酯0.0030.002氯氰菊酯0.000 50.000 1
    异菌脲0.0020.001溴氰菊酯0.000 70.001氰戊菊酯0.000 50.002
    下载: 导出CSV

    表  3  茄子样品的平均回收率和相对标准偏差(n=3)

    Table  3.   Average recoveries and RSDs of eggplant sample (n=3)

    %
    农药名称添加0.04 mg/Kg添加0.08 mg/Kg添加0.4 mg/Kg
    NY/T 761-2008QuEChERSNY/T 761-2008QuEChERSNY/T 761-2008QuEChERS
    回收率RSD回收率RSD回收率RSD回收率RSD回收率RSD回收率RSD
    六六六97.86.8104.13.2854.494.33.492.95.9111.37.6
    百菌清88.28.292.519.187.83.5106.65.7934.5107.34.9
    乙烯菌核利87.11.6102.513.879.61.172.12.580.33.392.36.9
    三唑酮82.32.5112.48.397.53.6113.17.1107.81.3109.63.2
    腐霉利125.33.188.88104.71.1123.96.888.4384.53.6
    异菌脲91.59.28714.2106.94.198.66107.58.685.71.5
    甲氰菊酯96.61.9112.31195.610.697.80.787.62.987.11.8
    三氟氯氰菊酯85.72.296.87.390.68.993.70.598.33101.21.9
    氟氯氰菊酯80.013.3101.513.989.16.4874.7105.63.3100.51.8
    氟氰戊菊酯96.64.6104.516.981.63.199.93.479.4396.12.3
    氟胺氰菊酯101.85.799.55.393.73.693.86.7102.53.61040.6
    溴氰菊酯107.56.699.64.8129.23.886.12.6106.33.694.60.5
    三氯杀螨醇95.17.878.86.798.16.391.515.3103.82.796.74.3
    滴滴涕85.34.876.37111.33.289.94.790.82.381.711.6
    联苯菊酯1106.4107.56.692.53.894393.83.7111.37.6
    氯菊酯108.25.792.811.883.84.293.28.8100.14.175.55.2
    氯氰菊酯113.55.781.315.298.85.4100.62.6100.13.7108.67.1
    氰戊菊酯1035.1103.915.1101.33.582.62100.34100.86.3
    下载: 导出CSV

    表  4  0.08 mg/Kg添加水平下Q法处理测定8个样品的回收率和相对标准偏差(n=3)

    Table  4.   Average recoveries and RSDs of adding 0.08 mg/Kg pesticides in 8 sample treated with QuEChERS (n=3)

    %
    农药名称菜豆茄子莴苣黄瓜结球甘蓝油桃马铃薯黄果柑
    回收
    RSD回收
    RSD回收
    RSD回收
    RSD回收
    RSD回收
    RSD回收
    RSD回收
    RSD
    六六六108.04.794.33.4102.72.785.02.195.35.093.46.682.54.375.91.7
    百菌清108.24.0106.65.793.04.9105.64.292.24.9111.63.0110.04.891.84.2
    乙烯菌核利113.07.472.12.572.12.591.57.587.43.799.39.084.49.494.14.9
    三唑酮116.43.2113.17.1116.23.1112.15.3107.33.590.92.898.85.3121.50.7
    腐霉利95.66.5123.96.8106.88.2101.42.9112.31.7111.013.2114.54.0113.12.3
    异菌脲89.64.398.66.097.97.091.12.793.94.893.32.695.65.294.76.0
    甲氰菊酯107.18.397.80.796.52.694.42.986.13.595.61.6102.75.977.511.4
    三氟氯氰菊酯112.97.193.70.591.83.494.63.885.33.594.42.399.14.683.32.7
    氟氯氰菊酯117.67.187.04.787.04.7107.42.6102.313.0104.92.1115.93.194.33.0
    氟氰戊菊酯105.617.199.93.499.93.4104.03.4103.111.9102.32.9117.45.3124.91.8
    氟胺氰菊酯98.89.893.86.793.86.7101.14.492.72.697.33.8117.84.790.84.0
    溴氰菊酯103.716.386.12.686.12.696.95.990.92.797.25.7113.23.084.45.5
    三氯杀螨醇99.07.291.515.392.41.3107.819.7105.75.9101.37.091.412.298.53.9
    滴滴涕97.39.289.94.793.92.880.118.897.51.882.23.591.82.185.45.8
    联苯菊酯107.68.394.03.084.73.498.015.3116.63.5110.65.6120.810.295.88.2
    氯菊酯97.012.093.28.878.53.694.44.784.76.8110.48.672.73.3102.92.0
    氯氰菊酯111.34.8100.62.697.55.499.46.288.13.0115.04.6105.64.296.92.7
    氰戊菊酯112.09.282.62.081.02.088.95.482.35.4112.98.980.67.791.82.0
    下载: 导出CSV
  • [1] 中华人民共和国农业部.NY/T 761-2008蔬菜和水果中有机磷、有机氯、拟除虫菊酯和氨基甲酸酯类农药多残留的测定[S].
    [2] Anastassiaeds Michelangelo, Lehotay Stajnbaher Darinka. Fast and easy multi residue method employing acetonitrile extraction /partitioning and dispersive solid-phase extraction for the determination of pesticide residues in product[J]. Journal of AOAC International, 2003, 86 (2):412-431.
    [3] 中华人民共和国农业部.NY/T 1380-2007蔬菜水果中51种农药多残留的测定气相色谱-质谱法[S].
    [4] Diez C, Traag W A, Zommer P, et al. Comparison of an acetonitrile extraction/partitioning and "dispersive solid-phaseextraction" method with classical multi-residue methods for the extraction of herbicide residues in barley samples[J]. Journal of Chromatography A, 2006, 1131: 11-23. doi: 10.1016/j.chroma.2006.07.046
    [5] 沈菁, 程运斌, 刘军, 等.分散固相萃取-高效液相色谱-质谱联用法测定大米中的呋喃丹残留[J].现代科学仪器, 2008 (2): 66-68. http://www.cnki.com.cn/Article/CJFDTOTAL-XDYQ200802022.htm
    [6] Aguilera-Luiz M M, Jose Luis Martinez Vidal, Roberto Romero-Gonzalez, et al. Multi-residue determination of veterinary drugs in milk by ultra-high-pressure liquid chromatography-tandem mass spectrometry[J]. Journal of Chromatography A, 2008, 1205: 10-16. doi: 10.1016/j.chroma.2008.07.066
    [7] Tomas Cajka, Jana Hajslova, Ondrej Lacina, et al. Rapid analysis of multi plepesticide residues in fruit-based baby food using programmed tempera-ture vaporizer injection-Low-pressure gas chromatography-high-resolution time-of-flight mass spectrometry[J]. Journal of Chromatography A, 2008, 1186: 281-294. doi: 10.1016/j.chroma.2007.12.009
    [8] 董静, 宫小明, 张立, 等. QuEChERS高效液相色谱法同时检测动物组织中的克球酚、地克珠利和磺胺类药物残留量[J].中国卫生检验杂志, 2008, 18(1): 26-29. http://www.cnki.com.cn/Article/CJFDTOTAL-ZWJZ200801012.htm
    [9] 郑文慧, 叶江雷, 王秀彬, 等.分散固相萃取法在农药残留检测中应用的进展[J].分析仪器, 2011(4):23-27. http://www.cnki.com.cn/Article/CJFDTOTAL-FXYQ201104019.htm
    [10] 林建, 薛晓康, 王露, 等.基质固相分散萃取气相质谱联用法测定蔬菜中六六六和滴滴涕农药残留[J].浙江农业科学, 2011(5):1131-1133. http://www.cnki.com.cn/Article/CJFDTOTAL-ZJNX201105061.htm
    [11] 刘亚伟, 董一威, 孙宝利, 等.QuEChERS在食品中农药多残留检测的应用研究进展[J].食品科学, 2009, 30(9):285-289. http://www.cnki.com.cn/Article/CJFDTOTAL-SPKX200909068.htm
    [12] 吴春梅, 程雪梅, 李亮, 等. QuEChERS-GPC-GC-MS快速测定蔬菜中24种农药残留[J].热带农业科学, 2012, 32(2):52-56. http://mall.cnki.net/magazine/Article/RDNK201202013.htm
    [13] 卢大胜, 熊丽蓓, 温忆敏, 等. QuEChERS前处理方法联合GPC-GC/MS在测定蔬菜水果农药残留中的应用[J].质谱学报, 2011, 4:229-235. http://mall.cnki.net/magazine/Article/ZPXB201104009.htm
    [14] Steven J Lehotay. Determination of pesticide residues in foods by acetointrile extraction and partitioning with magnesium sulfate:collaborative study [J]. Journal of AOAC International, 2007(90):485-520. http://cn.bing.com/academic/profile?id=2397819773&encoded=0&v=paper_preview&mkt=zh-cn
    [15] 中华人民共和国农业部.NY/T 789-2004农药残留分析样本的采样方法[S].
    [16] 国家质量监督局检验检疫总局.JJF 1059.1-2012测量不确定度评定与表示[S].
    [17] 国家质量技术监督局.JJF 1135-2005化学分析测量不确定度评定[S].
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  • 收稿日期:  2016-04-27
  • 修回日期:  2016-06-30
  • 刊出日期:  2016-09-01

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