GC-MS法快速筛查除草剂中非法添加成分
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摘要
[目的]应用气相色谱质谱联用仪建立了农药中12种常见非法添加除草剂成分的快速筛查方法,并对农药产品进行了分析。[方法]可湿性粉剂和乳油2种剂型的除草剂样品经丙酮或甲醇溶解,提取后采用GC-MS检测。[结果]12种常见非法添加除草剂在0.05～10mg/L质量浓度范围内具有良好的线性关系,相关系数均大于0.995,定量限均小于1.0mg/kg,目标物在农药基质中的回收率为90.8%～126.4%,相对标准偏差为1.0%～10.8%。[结论]该方法分析快速、灵敏、操作简单,测定结果具有较高的准确度和精密度,适用于除草剂中非法添加成分的筛查和定量测定。
[Aims] To establish a method for the simultaneous detection of 12 illegally added ingredients in herbicide products by gas chromatography-mass spectrometry(GC-MS) and analyze the pesticide samples. [Methods] The herbicides of wettable powder and emulsifiable concentrate were extracted with methanol or acetone, then detected by GC-MS. [Results] Twelve illegally added herbicides showed good linearity in the ranges of 0.05-10 mg/L, the correlation coefficients were higher than 0.995, the limits of detection were less than 1.0 mg/kg. The average recoveries were 90.8-126.4%, and the relative standard deviations were 1.0-10.8%. [Conclusions] The method is simple, rapid,sensitive and precision accuracy, and can be applied to screening and analysis of illegally added ingredients in herbicides.
[Aims] To establish a method for the simultaneous detection of 12 illegally added ingredients in herbicide products by gas chromatography-mass spectrometry(GC-MS) and analyze the pesticide samples. [Methods] The herbicides of wettable powder and emulsifiable concentrate were extracted with methanol or acetone, then detected by GC-MS. [Results] Twelve illegally added herbicides showed good linearity in the ranges of 0.05-10 mg/L, the correlation coefficients were higher than 0.995, the limits of detection were less than 1.0 mg/kg. The average recoveries were 90.8-126.4%, and the relative standard deviations were 1.0-10.8%. [Conclusions] The method is simple, rapid,sensitive and precision accuracy, and can be applied to screening and analysis of illegally added ingredients in herbicides.
引文
[1]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(1):21-23.
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[3]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.
[4]乔成奎,黄玉南,罗静,等.HPLC-MS/MS法检测农药产品中30种隐性成分[J].农药,2015,54(5):340-342.
[5]陈建波,吴爱娟,赵莉,等.超高效液相色谱-四级杆-飞行时间质谱法快速筛查农药制剂中非法添加的化学杀菌剂[J].分析化学,2017,45(3):441-447.
[6]陈建波,马琳,黄兰淇,等.超高效液相色谱-四级杆-飞行时间质谱法快速筛查农药制剂中非法添加的杀虫剂[J].色谱,2016,34(9):880-887.
[7]李建兵,王建萍,孙娜,等.农药中非法添加成分检测方法的研究进展[J].农药,2018,57(3):157-161.
[8]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.s
[2]林塬,吉哲蓉,王焱,等.气相色谱法同时测定不同农药产品中9种禁限用农药[J].农药,2018,57(10):735-738.
[3]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.
[4]乔成奎,黄玉南,罗静,等.HPLC-MS/MS法检测农药产品中30种隐性成分[J].农药,2015,54(5):340-342.
[5]陈建波,吴爱娟,赵莉,等.超高效液相色谱-四级杆-飞行时间质谱法快速筛查农药制剂中非法添加的化学杀菌剂[J].分析化学,2017,45(3):441-447.
[6]陈建波,马琳,黄兰淇,等.超高效液相色谱-四级杆-飞行时间质谱法快速筛查农药制剂中非法添加的杀虫剂[J].色谱,2016,34(9):880-887.
[7]李建兵,王建萍,孙娜,等.农药中非法添加成分检测方法的研究进展[J].农药,2018,57(3):157-161.
[8]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.s