固相萃取-气相色谱法检测齿瓣石斛中4种有机磷农药残留  

Determination of 4 Organophosphorus Dendrobium DevonianumPaxton in Dendrobium Dentata by Solid Phase Extraction andGas Chromatography

作　　者：柴连周[1] 刘超 郭妮 董寿堂[1] CHAI Lian-zhou;LIU Chao;GUO Ni;DONG Shou-tang(Baoshan College Of Traditional Chinese Medicine,Baoshan Yunnan 678000,China;Baoshan Comprehensive Inspection Centre of Quality and Technical Supervision,Baoshan Yunnan 678000,China)

机构地区：[1]保山中医药高等专科学校,云南宝山678000 [2]保山市质量技术监督综合检测中心,云南保山678000

出　　处：《粘接》2020年第5期56-58,共3页Adhesion

基　　金：云南省教育厅研究项目(2018JS649)。

摘　　要：目的:探索一种基于固相萃取净化--气相色谱法同时检测齿瓣石斛中4种有机磷类农药残留的方法,以期为齿瓣石斛的种植及产品开发提供技术参考。方法:以乙腈为提取溶剂,超声辅助提取,提取液经CARB固相萃取柱净化后,采用配有火焰光度检测器(FPD)、ZB-17毛细管色谱柱的气相色谱仪,通过柱程序升温进行检测,外标法定量。结果:检测结果表明4种有机磷农药的分离效果较好,且残留量在0.01~0.5μg/mL范围内有良好的线性关系,相关系数在0.9996~0.9999的范围内,加标回收率范围在84.83%~99.13%之间,RSD%(n=6)小于8%,检出限小于0.02mg/kg。结论:此方法可应用于同时检测齿瓣石斛中4种有机磷农药的残留,且符合行业标准。Objective:To explore a method for simultaneous determination of 4 organophosphorus pesticides in dendrobium devonianum paxton by solid phase extraction and gas chromatography,in order to provide a techni⁃cal reference for the planting and product development of dendrobium dendrobium paxton.Method:Acetonitrile was used as the extraction solvent and ultrasonic assisted extraction.After the extraction liquid was purified by CARB solid phase extraction column,a gas chromatograph equipped with a flame photometric detector(FPD)and a ZB-17 capillary chromatography column was used to detect the temperature by column programming and quantified by external standard method.Results:The test results showed that the separation effect of the four or⁃ganophosphorus pesticides was good.The regression equation of residues showed a good linear relationship with⁃in 0.01—0.5μg/mL with the correlation coefficients were within 0.9996—0.9999.The recoveries of all pesticides were between 81.39%—108.73%,and relative standard deviations RSD%(n=6)were less than 8%.The detec⁃tion limit is less than 0.02 mg/kg.Conclusion:This method can be used to detect organophosphorus pesticide resi⁃dues in dendrobium dendrobium simultaneously,which complies with industry standards.

关 键 词：齿瓣石斛 气相色谱法 有机磷农药 残留 

分 类 号：TQ450[化学工程—农药化工] O657.71A[理学—分析化学]