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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: To establish a method for the determination of five pyrethroid pesticide residues of flucythrinate, fenvalerate, beta-cypermethrin, permethrin, and bifenthrin in Lonicera japonica Thunb using liquid-liquid microextraction-high performance liquid chromatography . Methods: Five kinds of pyrethroid pesticides in honeysuckle were enriched with acetonitrile as dispersant and chloroform as extractant, and the factors influencing the efficiency of enrichment were optimized. The HPLC analysis was carried out on an Agilent ZORBAX XDB-C18 column (4.6 mm × 250 mm, 5μm). The mobile phase was eluted with acetonitrile-water. The detection wavelength was 230 nm and the flow rate was 1 mL · min-1. Results: The linear relationship between flufenthrin, fenvalerate, beta-cypermethrin, permethrin and bifenthrin was good (r> 0.999 0) at 0.05-5.0 mg · L -1, and the enrichment factor was between 18.6 ~ 29.7, high, medium and low concentration of three kinds of average recovery rate of 72.1% ~ 110.4%. Conclusion: The method is simple, accurate, sensitive and can meet the requirements of pyrethroid pesticide residue analysis.