微波萃取-高效液相色谱法测定稻谷中敌敌畏的残留量
Determination of dichlorovos residue in rice by microwave-assisted extraction/HPLC
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摘要: 目的: 建立了微波辅助萃取-高效液相色谱法测定稻谷中敌敌畏残留量的方法。 方法: 以丙酮-乙腈(体积比3:7)为提取剂,采用微波辅助萃取稻谷中残留的敌敌畏,经弗罗里硅土及中性氧化铝柱层析净化,以乙腈-水为流动相,流速1.0 mL/min,200 nm检测。 结果: 敌敌畏在2.0-25.0μg/mL范围内呈良好的线性关系,检测限为0.5μg/mL,稻壳添加平均回收率为81.1%,RSD为3.9%;糙米添加平均回收率为78.9%,RSD为4.0%。 结论: 该方法简便、快速,可用于稻谷中敌敌畏残留量的测定。Abstract: Objective: To develop a method of microwave-assisted extraction（MAE）followed by HPLC for the determination of the residue of dichlorovos in rice. Methods: Pesticide residues were extracted from rice samples with a solvent mixture.Extracts were cleaned up with a column filled with Florisil and neutral aluminum oxide.Nova-Pak C18 column（4 μm,3.9×150 mm）was used with acetonitrile:water（3070,V/V）solution as mobile phase,and the flow speed was 1.0mL/min.The ultraviolet detection wavelength was 200nm. Results: Good linear correlation for dichlorovos was found in the concentration range of 2.00-25.00 μg/mL.The detection limit was 0.5 μg/mL for dichlorovos（S/N=3）.The average recovery rate of rice hull and brown rice were 81.1%（RSD3.9%） and 78.9%（RSD4.0%）,respectively. Conclusion: This method is simple and rapid.It can be used for the determination of dichlorovos residue in rice with satisfactory results.
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Key words:
- microwave-assisted extraction /
- HPLC /
- dichlorovos /
- rice hull /
- brown rice
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