超高效液相色谱-串联质谱法检测番茄和甘蓝中溴虫氟苯双酰胺的残留
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摘要
[目的]利用超高效液相色谱-串联质谱建立番茄和甘蓝中溴虫氟苯双酰胺残留量测定的方法。[方法]样品用酸化乙腈提取,N-丙基乙二胺分散吸附剂净化,超高效液相色谱分离,三重四级杆串联质谱检测,外标法定量。[结果]溴虫氟苯双酰胺在0.0002～0.2 mg/L质量浓度范围内呈现出良好的线性关系(r>0.999),当添加质量分数为0.01～0.5 mg/kg时,溴虫氟苯双酰胺在番茄中的平均回收率为71.9%～97.3%,相对标准偏差为3.2%～4.1%;在甘蓝中的平均回收率为77.5%～117.5%,相对标准偏差为6.4%～7.6%。[结论]方法的灵敏度、准确度、精密度符合农药残留分析的要求。
[Aims ] A rapid and sensitive analytical method for detecting broflanilide residues in tomato and cabbage samples was established. [Me thods ] The sample was extracted with acid acetonitrile, subsequently cleaned-up with primary secondary amine prior to sample analysis. UPLC-MS/MS operated on positive ionization and detected in multi-reaction monitoring model, quantitative by external standard method. [Re s ults ] The method showed excellent linearity(r>0.999) for broflanilide in the range of 0.0002-0.02 mg/L. Recovery studies were performed at spiked levels of 0.01-0.5 mg/kg. Recoveries of the method ranged from 71.9 to 97.3% with relative standard deviation(RSD) ranged from 3.2 to 4.1% for tomato at different levels. Recoveries for cabbage at different levels ranged from 77.5 to 117.5%with RSD ranged from 6.4 to 7.6%. [Conclus ions ] The method was simple and reliable, meet with the requirement of pesticide residues analysis, and could be applied for determining broflanilide in tomato and cabbage.
[Aims ] A rapid and sensitive analytical method for detecting broflanilide residues in tomato and cabbage samples was established. [Me thods ] The sample was extracted with acid acetonitrile, subsequently cleaned-up with primary secondary amine prior to sample analysis. UPLC-MS/MS operated on positive ionization and detected in multi-reaction monitoring model, quantitative by external standard method. [Re s ults ] The method showed excellent linearity(r>0.999) for broflanilide in the range of 0.0002-0.02 mg/L. Recovery studies were performed at spiked levels of 0.01-0.5 mg/kg. Recoveries of the method ranged from 71.9 to 97.3% with relative standard deviation(RSD) ranged from 3.2 to 4.1% for tomato at different levels. Recoveries for cabbage at different levels ranged from 77.5 to 117.5%with RSD ranged from 6.4 to 7.6%. [Conclus ions ] The method was simple and reliable, meet with the requirement of pesticide residues analysis, and could be applied for determining broflanilide in tomato and cabbage.
引文
[1]NAKAO T,BANBA S.Broflanilide:A Meta-diamide Insecticide with a Novel Mode of Action[J].Bioorganic&Medicinal Chemistry,2016,24(3):372-377.
[2]齐浩亮,崔丽,王芹芹,等.溴虫氟苯双酰胺对小菜蛾的毒力及相关酶活性的影响[J].植物保护,2017,43(1):112-116.
[3]朱洪伟,王胜翔,郭海霞.溴虫氟苯双酰胺悬浮剂毛细管气相色谱分析方法研究[J].农药科学与管理,2015(36):1-3.
[4]徐赛,韩冲冲,李飞,等.5%溴虫氟苯双酰胺悬浮剂的高效液相色谱分析方法[J].农药,2018,57(1):29-30.
[5]NY/T 788-2018.农作物中农药残留试验准则[S].北京:中国标准出版社,2018.
[6]VAN EECKHAUT A,LANCKMANS K,SARRE S,et al.Validation of Bioanalytical LC-MS/MS Assays:Evaluation of Matrix Effects[J].Journal of Chromatography B,2009,877(23):2198-2207
[7]LI Min-min,LIU Xin-gang,DONG Feng-shou,et al.Simultaneous Determination of Cyflumetofen and Its Main Metabolite Residues in Samples of Plant and Animal Origin Using Multi-walled Carbon Nanotubes in Dispersive Solid-phase Extraction and Ultrahigh Performance Liquid Chromatographytandem Mass Spectrometry[J].Journal of Chromatography A,2013,1300:95-103.
[2]齐浩亮,崔丽,王芹芹,等.溴虫氟苯双酰胺对小菜蛾的毒力及相关酶活性的影响[J].植物保护,2017,43(1):112-116.
[3]朱洪伟,王胜翔,郭海霞.溴虫氟苯双酰胺悬浮剂毛细管气相色谱分析方法研究[J].农药科学与管理,2015(36):1-3.
[4]徐赛,韩冲冲,李飞,等.5%溴虫氟苯双酰胺悬浮剂的高效液相色谱分析方法[J].农药,2018,57(1):29-30.
[5]NY/T 788-2018.农作物中农药残留试验准则[S].北京:中国标准出版社,2018.
[6]VAN EECKHAUT A,LANCKMANS K,SARRE S,et al.Validation of Bioanalytical LC-MS/MS Assays:Evaluation of Matrix Effects[J].Journal of Chromatography B,2009,877(23):2198-2207
[7]LI Min-min,LIU Xin-gang,DONG Feng-shou,et al.Simultaneous Determination of Cyflumetofen and Its Main Metabolite Residues in Samples of Plant and Animal Origin Using Multi-walled Carbon Nanotubes in Dispersive Solid-phase Extraction and Ultrahigh Performance Liquid Chromatographytandem Mass Spectrometry[J].Journal of Chromatography A,2013,1300:95-103.