固相萃取-双柱双检测器-气相色谱法测定蔬菜中55种有机磷农药残留  

Determination of organophosphorous pesticides in vegetables by dual-column-dual-detector-gas chromatography

作　　者：李继革[1] 王玉飞[1] 范建中[1] 施家威[1] 赵永纲[1] 

机构地区：[1]宁波市疾病预防控制中心宁波市毒物研究与控制重点实验室,浙江宁波315010

出　　处：《中国卫生检验杂志》2010年第11期2711-2715,共5页Chinese Journal of Health Laboratory Technology

摘　　要：目的:建立了固相萃取-双柱双检测器-气相色谱法测定蔬菜中多种有机磷农药残留的方法。方法:样品中的有机磷农药经乙腈-丙酮混合溶剂匀浆提取,Carb-NH2固相萃取柱净化,DB-1701柱分离后进入FPD检测器进行定性定量、HP-5分离后进入NPD检测器进行验证。结果:在0.5μg/ml～10.0μg/ml范围内质量浓度与峰面积有良好的线性关系,加标回收率在70%～124%之间,相对标准偏差(RSD)在2.31%～10.4%,方法检测限在0.005 mg/kg～0.030 mg/kg。结论:该方法充分利用双柱定性的优势,检测结果准确、可靠,达到农残检测的要求,适用蔬菜中多种有机磷的同时测定。Objective：A method for the determination of organophosphorous pesticide residues in vegetables by solid phase extraction（SPE） coupled with dual-column-dual-detector-gas chromatography（GC） was developed and validated.Methods： The samples were extracted by acetonitrile-acetone and purificated with Carb-NH2 SPE column,then detected by DB-1701-FPD and HP-5-NPD,respectively.Results： The results demonstrated that the linear ranges were 0.5 μg/ml～10.0 μg/ml.The average recoveries ranged from 70% to 124% with the relative standard deviations of 2.31%～10.4% at the spiking levels of 0.05 mg/kg,0.10 mg/kg and 0.60 mg/kg in vegetable samples,the limits of detection were 0.005 mg/kg～0.030 mg/kg.Conclusion： This method is accurate,sensitive and suitable for the analysis of pesticide residues in vegetables.

关 键 词：固相萃取 双柱双检测器 气相色谱 有机磷 

分 类 号：TS207.53[轻工技术与工程—食品科学]