[Objectives]This study was conducted to purify mutton samples by gel permeation chromatography(GPC).[Methods]Fourteen organophosphorus pesticide residues in samples were qualitatively and quantitatively analyzed by ga...[Objectives]This study was conducted to purify mutton samples by gel permeation chromatography(GPC).[Methods]Fourteen organophosphorus pesticide residues in samples were qualitatively and quantitatively analyzed by gas chromatography-mass spectrometry(GC-MS)in selective ion scanning mode(SIM).[Results]The organophosphorus pesticide standard solutions showed good linearity in the mass concentration range of 0.1-10.0μg/ml with correlation coefficients(r)not lower than 0.999,and the detection limits(S=3 N)ranged from 0.01 to 0.05 mg/kg.The average recovery values were in the range of 80.2%-99.7%,with relative standard deviations(RSDs,n=3)in the range of 1.8%-6.3%,at the addition levels of 0.5,1.0 and 2.0 mg/kg.[Conclusions]The method is simple,sensitive and accurate,and can be used for the determination of organophosphorus pesticide residues in mutton.展开更多
目的:基于QuEChERS方法结合气相色谱串联质谱(Gas Chromatography-Tandem Mass Spectrometry,GC-MS/MS)技术,建立一种简单、快速检测果蔬中农药残留的方法。方法:果蔬样品匀浆后,先用乙腈和乙酸缓冲盐包提取,再用m-PFC小柱净化,最后用GC...目的:基于QuEChERS方法结合气相色谱串联质谱(Gas Chromatography-Tandem Mass Spectrometry,GC-MS/MS)技术,建立一种简单、快速检测果蔬中农药残留的方法。方法:果蔬样品匀浆后,先用乙腈和乙酸缓冲盐包提取,再用m-PFC小柱净化,最后用GC-MS/MS测定,外标法定量。结果:13种农药在10~500μg·L^(-1)浓度范围内线性关系良好,相关系数(R^(2))均大于0.994,检出限为0.35~0.92μg·kg^(-1),定量限为1.0~2.8μg·kg^(-1);13种农药在3个水平下的加标回收率为82.4%~110.1%,相对标准偏差为2.9%~9.3%。结论:所建立的方法可操作性强,具有较高的精密度和准确度,可用于果蔬中农药残留的定性和定量检测。展开更多
油料作物由于含油量高、基质复杂,导致其弱极性多环芳烃类化合物提取率低,成为准确检测高油样品中多环芳烃的瓶颈。本文对比了16种多环芳烃的GC-MS/MS检测条件SIM(Single Ion Monitoring)模式和SRM(Selective Reaction Monitoring)模式...油料作物由于含油量高、基质复杂,导致其弱极性多环芳烃类化合物提取率低,成为准确检测高油样品中多环芳烃的瓶颈。本文对比了16种多环芳烃的GC-MS/MS检测条件SIM(Single Ion Monitoring)模式和SRM(Selective Reaction Monitoring)模式质谱信号响应,SRM模式干扰峰更少,检出限更低;对比了QuEChERS和超声辅助提取方法对大豆、油菜籽、花生三种油料中16种多环芳烃的提取效果,超声辅助提取的基质效应很高,部分多环芳烃基质减弱80%以上,且油菜籽的提取稳定性差,部分相对标准偏差达到32%~45%。并比较了乙腈和丙酮作为QuCEhERS方法提取溶剂的提取效果。结果表明,QuCEhERS方法中乙腈作为提取溶剂,在极性最弱的多环芳烃回收率低,如苯并[b]荧蒽、苯并[k]荧蒽等,回收率甚至小于10%。而丙酮作为QuCEhERS方法提取溶剂,而在极性弱的多环芳烃中,回收率提高了3~5倍,适合提取高油样品中多环芳烃。三种油料基质匹配标准曲线的相关系数均在0.99以上。16种多环芳烃均能获得较好的回收率(58%~100%),相对标准偏差为0.4%~10.6%,方法稳定性好。展开更多
基金Supported by The Fourth Batch of High-end Talent Project in Hebei Province.
文摘[Objectives]This study was conducted to purify mutton samples by gel permeation chromatography(GPC).[Methods]Fourteen organophosphorus pesticide residues in samples were qualitatively and quantitatively analyzed by gas chromatography-mass spectrometry(GC-MS)in selective ion scanning mode(SIM).[Results]The organophosphorus pesticide standard solutions showed good linearity in the mass concentration range of 0.1-10.0μg/ml with correlation coefficients(r)not lower than 0.999,and the detection limits(S=3 N)ranged from 0.01 to 0.05 mg/kg.The average recovery values were in the range of 80.2%-99.7%,with relative standard deviations(RSDs,n=3)in the range of 1.8%-6.3%,at the addition levels of 0.5,1.0 and 2.0 mg/kg.[Conclusions]The method is simple,sensitive and accurate,and can be used for the determination of organophosphorus pesticide residues in mutton.
文摘目的:基于QuEChERS方法结合气相色谱串联质谱(Gas Chromatography-Tandem Mass Spectrometry,GC-MS/MS)技术,建立一种简单、快速检测果蔬中农药残留的方法。方法:果蔬样品匀浆后,先用乙腈和乙酸缓冲盐包提取,再用m-PFC小柱净化,最后用GC-MS/MS测定,外标法定量。结果:13种农药在10~500μg·L^(-1)浓度范围内线性关系良好,相关系数(R^(2))均大于0.994,检出限为0.35~0.92μg·kg^(-1),定量限为1.0~2.8μg·kg^(-1);13种农药在3个水平下的加标回收率为82.4%~110.1%,相对标准偏差为2.9%~9.3%。结论:所建立的方法可操作性强,具有较高的精密度和准确度,可用于果蔬中农药残留的定性和定量检测。
文摘油料作物由于含油量高、基质复杂,导致其弱极性多环芳烃类化合物提取率低,成为准确检测高油样品中多环芳烃的瓶颈。本文对比了16种多环芳烃的GC-MS/MS检测条件SIM(Single Ion Monitoring)模式和SRM(Selective Reaction Monitoring)模式质谱信号响应,SRM模式干扰峰更少,检出限更低;对比了QuEChERS和超声辅助提取方法对大豆、油菜籽、花生三种油料中16种多环芳烃的提取效果,超声辅助提取的基质效应很高,部分多环芳烃基质减弱80%以上,且油菜籽的提取稳定性差,部分相对标准偏差达到32%~45%。并比较了乙腈和丙酮作为QuCEhERS方法提取溶剂的提取效果。结果表明,QuCEhERS方法中乙腈作为提取溶剂,在极性最弱的多环芳烃回收率低,如苯并[b]荧蒽、苯并[k]荧蒽等,回收率甚至小于10%。而丙酮作为QuCEhERS方法提取溶剂,而在极性弱的多环芳烃中,回收率提高了3~5倍,适合提取高油样品中多环芳烃。三种油料基质匹配标准曲线的相关系数均在0.99以上。16种多环芳烃均能获得较好的回收率(58%~100%),相对标准偏差为0.4%~10.6%,方法稳定性好。
