液相色谱-串联质谱法测定果蔬中双三氟虫脲、四氯虫酰胺和氰虫酰胺残留
发布时间：2018-11-25 12:32
【摘要】：建立了蔬菜和水果中双三氟虫脲、四氯虫酰胺和氰虫酰胺3种新型杀虫剂的分散固相萃取-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C18基质分散净化剂进行净化,液相色谱-三重四极杆串联质谱(LC-MS/MS)同时进行检测。双三氟虫脲和四氯虫酰胺采用多反应监测负离子模式,氰虫酰胺采用多反应监测正离子模式。双三氟虫脲在苹果、洋葱和经微波处理的洋葱样品中均不存在基质效应,可采用纯溶剂标准外标法或者采用基质匹配标准溶液定量检测;四氯虫酰胺和氰虫酰胺存在程度不同的基质减弱效应,采用空白基质匹配的校正标准曲线外标法定量。3种杀虫剂均在0.2~100μg/L线性范围内具有良好的线性关系,相关系数均大于0.9990。在0.005~2.000 mg/kg范围内,平均添加回收率为81.6%~99.9%,相对标准偏差为3.6%~9.8%。氰虫酰胺、四氯虫酰胺和双三氟虫脲的检出限分别为0.064,0.048和0.001μg/kg,定量限分别为0.210,0.160和0.004μg/kg。
[Abstract]:A method for the determination of three new insecticides in vegetables and fruits by dispersive solid-phase extraction-liquid chromatography-tandem mass spectrometry was developed. The samples were extracted by acetonitrile homogenization and purified by ethylenediamine-N-propylsilane (PSA) and C18 matrix dispersion purifier. The samples were detected by liquid chromatography-triple quadrupole tandem mass spectrometry (LC-MS/MS). The negative ion pattern was monitored by multi-reaction and the positive ion pattern was monitored by multi-reaction of dichloromide and tetrachloromide. There was no matrix effect in apple, onion and microwave treated onion samples, which could be detected by standard external standard method of pure solvent or matrix matching standard solution. The matrix weakening effect of tetrachloromide and cyanamide was different. The calibration standard curve external standard method for blank matrix matching was used to quantify the three insecticides. There was a good linear relationship in the linear range of 0.2 渭 g / L for all three insecticides. The correlation coefficient is more than 0.9990. In the range of 0.005 ~ 2.000 mg/kg, the average recovery was 81.6 ~ 99.9 and the relative standard deviation was 3.6 ~ 9.8. The detection limits of cyandiamide, tetrachloromide and dichloromide were 0.064 渭 g / kg and 0.001 渭 g / kg, respectively, and the quantification limits were 0.210 渭 g / kg and 0.004 渭 g / kg, respectively.
【作者单位】： 山东出入境检验检疫局检验检疫技术中心;山东省农业科学院植物保护研究所;
【基金】：山东出入境检验检疫科研项目(No.SK201425)资助
【分类号】：TS255.7;O657.63
本文编号：2356116
[Abstract]:A method for the determination of three new insecticides in vegetables and fruits by dispersive solid-phase extraction-liquid chromatography-tandem mass spectrometry was developed. The samples were extracted by acetonitrile homogenization and purified by ethylenediamine-N-propylsilane (PSA) and C18 matrix dispersion purifier. The samples were detected by liquid chromatography-triple quadrupole tandem mass spectrometry (LC-MS/MS). The negative ion pattern was monitored by multi-reaction and the positive ion pattern was monitored by multi-reaction of dichloromide and tetrachloromide. There was no matrix effect in apple, onion and microwave treated onion samples, which could be detected by standard external standard method of pure solvent or matrix matching standard solution. The matrix weakening effect of tetrachloromide and cyanamide was different. The calibration standard curve external standard method for blank matrix matching was used to quantify the three insecticides. There was a good linear relationship in the linear range of 0.2 渭 g / L for all three insecticides. The correlation coefficient is more than 0.9990. In the range of 0.005 ~ 2.000 mg/kg, the average recovery was 81.6 ~ 99.9 and the relative standard deviation was 3.6 ~ 9.8. The detection limits of cyandiamide, tetrachloromide and dichloromide were 0.064 渭 g / kg and 0.001 渭 g / kg, respectively, and the quantification limits were 0.210 渭 g / kg and 0.004 渭 g / kg, respectively.
【作者单位】： 山东出入境检验检疫局检验检疫技术中心;山东省农业科学院植物保护研究所;
【基金】：山东出入境检验检疫科研项目(No.SK201425)资助
【分类号】：TS255.7;O657.63
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