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分散液液微萃取-高效液相色谱法测定金银花中拟除虫菊酯类农药残留 被引量:9

Determination of Pyrethroid Pesticide Residues in Lonicerae Janponicae Flos by Disperse Liquid-liquid Microextraction Coupled with HPLC
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摘要 目的:建立分散液液微萃取-高效液相色谱法测定金银花中氟氰戊菊酯、氰戊菊酯、高效氟氯氰菊酯、氯菊酯、联苯菊酯5种拟除虫菊酯类农药残留的方法.方法:以乙腈为分散剂,三氯甲烷为萃取剂富集金银花中5种菊酯类农药,并优化影响富集效率的因素;采用HPLC测定,Agilent ZORBAX XDB-C18色谱柱(4.6 mm×250 mm,5μm),流动相乙腈-水梯度洗脱,检测波长230 nm,流速1 mL· min^-1.结果:氟氰戊菊酯、氰戊菊酯、高效氟氯氰菊酯、氯菊酯、联苯菊酯在0.05 ~5.0 mg·L^-1线性关系良好(r >0.999 0),富集倍数在18.6 ~29.7,高、中、低3种浓度平均加样回收率在72.1% ~ 110.4%.结论:该方法操作简便、准确性好,灵敏度高,可满足菊酯类农药残留分析的要求. Objective:This study was aimed to establish disperse liquid-liquid microextraction coupled with high performance liquid chromatography (DLLME-HPLC) method for determination of five pyrethroid pesticides (flucythrinate,fenvalerate,lambda-cyhalothrin,permethrin,bifenthrin) in Lonicerae Janponicae Flos.Method:The five pyrethroid pesticides in Lonicerae Janponicae Flos were extracted by trichlormethane,with acetonitrile as dispersant,then analysed by HPLC.Some important parameters that influenced the extraction efficiency were optimized.The five pesticides were separated by an Agilent ZORBAX XDB-C18 (4.6 mm × 250 mm,5 μm) column in the wavelength at 230 nm.The mobile phase was acetonitrile-H2O with gradient elution and the flow rate was 1.0 mL · min-1 Result:Flucythrinate,fenvalerate,lambda-cyhalothrin,permethrin and bifenthrin showed good linear relation within range of 0.05-5.0 mg ·L^-1 (r 〉 0.999 0).The enrichment factors ranged from 18.6 to 29.7.The average recovery of high,medium and low concentration ranged from 72.1% to 110.4%,Conclusion:The method is accurate and sensitive,simple and fast,and can meet the requirement of pyrethroid pesticedes residue analysis in Lonicerae Janponicae Flos.
作者 周卿 周旭美
出处 《中国实验方剂学杂志》 CAS 北大核心 2014年第20期70-73,共4页 Chinese Journal of Experimental Traditional Medical Formulae
基金 贵州省中医药管理局项目(QZYY2012-D406)
关键词 金银花 菊酯类农药 分散液液微萃取 高效液相色谱法 Lonicerae Janponicae Flos pyrethroid pesticedes disperse liquid-liquid microextraction HPLC
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