气相色谱法同时测定不同农药产品中9种禁限用农药
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摘要
[目的]应用气相色谱仪建立7种农药制剂产品中9种禁限用农药的检测方法,并对农药样品进行分析。[方法]试验采用超声提取法和气相色谱法进行研究。[结果]通过提取溶剂和超声提取时间的优化,确定以丙酮为提取溶液,超声时间10 min。所检测的9种禁限用农药在0.5～5.0 mg/L质量浓度范围内具有良好的线性关系,相关系数R2为0.9982～0.9999,最低检出限为0.02～0.03 mg/kg,目标物在农药基质中的平均回收率为80.42%～113.06%,相对标准偏差为0.64%～8.35%。[结论]该方法具有操作简单、分离效果好、检测限低、回收率高等优点。
[Aims] To establish a method for the simultaneous detection of 9 forbidden and limiting pesticides in7 pesticide products by gas chromatography and analyze the pesticide sample. [Methods] Ultrasonic extraction and gas chromatography were used for the study. [Results] Through the optimization of extraction solvent and ultrasonic extraction time, acetone was used as the extraction solution and the ultrasonic extraction time was 10 min. Nine forbidden and limiting pesticides showed good linearity in the ranges of 0.5-5.0 mg/L, the correlation coefficient R~2 was0.9982-0.9999, the limits of detection(LOD) were 0.02-0.03 mg/kg. The average recoveries were 80.42-113.06%, and the relative standard deviations(RSD) were 0.64-8.35%. [Conclusions] The method is easy to operate and has the advantages of good separation effect, low limit of detection and good recovery rate.
[Aims] To establish a method for the simultaneous detection of 9 forbidden and limiting pesticides in7 pesticide products by gas chromatography and analyze the pesticide sample. [Methods] Ultrasonic extraction and gas chromatography were used for the study. [Results] Through the optimization of extraction solvent and ultrasonic extraction time, acetone was used as the extraction solution and the ultrasonic extraction time was 10 min. Nine forbidden and limiting pesticides showed good linearity in the ranges of 0.5-5.0 mg/L, the correlation coefficient R~2 was0.9982-0.9999, the limits of detection(LOD) were 0.02-0.03 mg/kg. The average recoveries were 80.42-113.06%, and the relative standard deviations(RSD) were 0.64-8.35%. [Conclusions] The method is easy to operate and has the advantages of good separation effect, low limit of detection and good recovery rate.
引文
[1]卜元卿,孔源,智勇,等.化学农药对环境的污染及其防控对策建议[J].中国农业科技导报, 2014, 16(2):19-25.
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[3]王威,贺红武,王列平,等.有机磷农药及其研发概况[J].农药,2016, 55(2):86-90.
[4]郭映花,杨惠芳.我国禁(限)用农药的管理与控制现状[J/OL].现代预防医学, 2013, 40(12):2198-2202.
[5]龚洁.农药隐性成分乱象丛生[N].农资导报, 2011-06-28(C01).
[6]吴利交.强化禁限用农药管理,保障农产品质量安全[J/OL].现代园艺, 2016(16):53-54.
[7]袁善奎,刘亮,王以燕,等.农药非法添加隐性成分及其风险分析[J].农药, 2016, 55(7):480-482, 490.
[8]洪华,张晓强,武中平,等. SPE-GC-MS快速定性定量杀虫剂产品中11种违禁添加菊酯类隐性成分[J].农药, 2013, 52(11):812-814.
[9]李海燕,施慧娟,肖峥.农药杀虫剂中11种禁限用农药的同时检测[J].上海计量测试, 2015, 42(1):21-23.
[2]汪建沃.禁用农药为何屡禁不绝[N].中国化工报, 2015-12-11(006).
[3]王威,贺红武,王列平,等.有机磷农药及其研发概况[J].农药,2016, 55(2):86-90.
[4]郭映花,杨惠芳.我国禁(限)用农药的管理与控制现状[J/OL].现代预防医学, 2013, 40(12):2198-2202.
[5]龚洁.农药隐性成分乱象丛生[N].农资导报, 2011-06-28(C01).
[6]吴利交.强化禁限用农药管理,保障农产品质量安全[J/OL].现代园艺, 2016(16):53-54.
[7]袁善奎,刘亮,王以燕,等.农药非法添加隐性成分及其风险分析[J].农药, 2016, 55(7):480-482, 490.
[8]洪华,张晓强,武中平,等. SPE-GC-MS快速定性定量杀虫剂产品中11种违禁添加菊酯类隐性成分[J].农药, 2013, 52(11):812-814.
[9]李海燕,施慧娟,肖峥.农药杀虫剂中11种禁限用农药的同时检测[J].上海计量测试, 2015, 42(1):21-23.