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液相色谱-串联质谱法测定果蔬中4种新型卵菌纲杀菌剂残留
Determination of New Type of 4 Bactericids Used for Control of Oomycete Diseases Residues in Fruits and Vegetables by Liquid Chromatography/Tandem Mass Spectrometry
【摘要】 建立了蔬菜和水果中噻唑菌胺、苯噻菌胺、氟啶酰菌胺和双炔酰菌胺4种新型卵菌纲杀菌剂的分散固相萃取-液相色谱-串联质谱检测方法。样品经乙腈均质提取,混合使用乙二胺-N-丙基硅烷(PSA)和ODSC18-N两种基质分散净化剂净化,采用液相色谱-三重四级杆串联质谱(LC/MS/MS)检测。实验通过空白基质溶液稀释标准建立校正的标准曲线,以消除基质效应。结果表明,噻唑菌胺和氟啶酰菌胺在1~100μg/L,苯噻菌胺和双炔酰菌胺在0.5~50μg/L线性范围内具有良好的线性关系,相关系数为0.9994~0.9999;4种卵菌纲杀菌剂添加回收率在80.9%~101.3%之间;相对标准偏差(RSD)均小于6.3%。定量限在0.53~1.3μg/kg之间,检出限为0.16~0.40μg/kg。
【Abstract】 A method was developed for the determination of ethaboxam,benthivalicarb-isopropyl,fluopicolide and mandipropamid in fruits and vegetables.The analytes were extracted from the samples by acetonitrile,and purified by dispersion solid phase extraction using ODS C18-N and PSA as solidphase,and then analyzed by LC/MS/MS with multiple reaction monitoring(MRM).The interference of matrix was reduced by the matrix-matched calibration standards curve.The linear range was from 1 μ /L to 100 μ /L for ethaboxam,fluopicolide,from 0.5 μ/L to 50 μ g/L for benthivalicarb-isopropyl,mandipropamid(r≥0.9994).The fortified recoveries were from 80.9% to 101.3% with relative standard deviations(RSD) lass than 6.3%.The limits of quantification were 0.53 μ g/kg to 1.3 μ g/kg and the limit of detection were 0.16 to 0.40 μ g/kg.
【Key words】 Liquid chromatography-tandem mass spectrometry; Fruits and vegetables; Ethaboxam; Fluopicolide; Benthivalicarb-isopropyl; Mandipropamid;
- 【文献出处】 分析化学 ,Chinese Journal of Analytical Chemistry , 编辑部邮箱 ,2011年12期
- 【分类号】TS255.7;TS255.7
- 【被引频次】16
- 【下载频次】370