气相色谱串联质谱法测定食用菌中拟除虫菊酯类农药
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摘要
目的建立食用菌中拟除虫菊酯类农药的GC/MS/MS测定方法。方法取切碎混匀的样品用乙腈提取,用Carb/NH2柱净化.浓缩液用氮气吹至近干后用1 mL丙酮准确定容,待GC/MS/MS分析。结果拟除虫菊酯类农药的色谱分离效果、线性方程相关性均良好,满足实验要求。其相关系数r=0.991 2～0.999 5,方法的检出限为0.001 mg/kg,定量限为0.003 mg/kg,回收率范围72.6%～88.2%。结论该方法方便、灵敏度高,适用于食用菌中拟除虫菊酯类农药的测定。
Objective To establish a rapid and accurate method for determination of Pyrethroid pesticides residue in edible fungi by gas chromatography-tandem mass spectrometry(GC-MS/MS). Methods The samples were extracted by acetonitrile, cleaned up by Carb/NH2 column and determined by GC-MS/MS. Results Under the optimized experimental conditions,the linearity and precision of the method were good and can meet the requirement of the test.The correlation coefficient was 0.991 2 ～0.999 5, Limits of detection and quantification for Pyrethroid pesticides residue were 0.001 mg/kg and 0.003 mg/kg, and the recoveries was 72.6 %～88.2 %. Conclusions This method is convenient,sensitivity and accurate. It is suitable for the qualitative and quantitative determination of Pyrethroid pesticides residue in edible fungi.
Objective To establish a rapid and accurate method for determination of Pyrethroid pesticides residue in edible fungi by gas chromatography-tandem mass spectrometry(GC-MS/MS). Methods The samples were extracted by acetonitrile, cleaned up by Carb/NH2 column and determined by GC-MS/MS. Results Under the optimized experimental conditions,the linearity and precision of the method were good and can meet the requirement of the test.The correlation coefficient was 0.991 2 ～0.999 5, Limits of detection and quantification for Pyrethroid pesticides residue were 0.001 mg/kg and 0.003 mg/kg, and the recoveries was 72.6 %～88.2 %. Conclusions This method is convenient,sensitivity and accurate. It is suitable for the qualitative and quantitative determination of Pyrethroid pesticides residue in edible fungi.
引文
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[7]田菲菲,张曦,马金凤,等.气相色谱-串联质谱法同时分析葡萄基质中196种农药残留[J].食品安全质量检测学报,2016,7(3):1071-1080.
[8]郑茜尹,陈璐莹,李强,等.免净-气相色谱串联质谱法测定大米59种农残[J].现代预防医学,2017,44(21):4000-4004.
[2]蒋梅峰,李鹏,余寅.气相色谱法同时测定小麦和玉米中氰戊菊酯、氯氰菊酯及溴氰菊酯类农药残留量[J].食品工程,2014,12(4):57-59.
[3]严明.拟除虫菊酯类农药的GCMSMS定性分析方法.广东公安科技,2010,101(4):12-14.
[4]王会锋,冯书惠,贾斌.40种农药残留量的气相色谱法测定[J].分析检测,2010,31(20):335-341.
[5]何彩.蔬菜中拟除虫菊酯类农药气质联用仪检测法[J].职业与健康,2010,26(15):1717-1718.
[6]蓝锦昌,徐敦明,周昱,等.加速溶剂萃取(ASE)气相色谱/串联质谱(GC/MS/MS)法测定食用菌中25种农药残留[J].分析应用科技,2010,37(5):56-64.
[7]田菲菲,张曦,马金凤,等.气相色谱-串联质谱法同时分析葡萄基质中196种农药残留[J].食品安全质量检测学报,2016,7(3):1071-1080.
[8]郑茜尹,陈璐莹,李强,等.免净-气相色谱串联质谱法测定大米59种农残[J].现代预防医学,2017,44(21):4000-4004.