高效液相色谱法同时检测稻田样品中5种除草剂的残留量
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农业部农药登记残留项目(2014H277)


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    摘要:

    建立一种高效液相色谱法同时检测稻田土壤、稻田水和糙米中二甲四氯、2,4,5–T、高效氟吡甲禾灵、精吡氟禾草灵和精喹禾灵5种除草剂残留的方法。土壤样品用0.05%磷酸溶液和乙腈混合液(体积比为1∶2)提取,水样品用乙酸乙酯萃取,糙米样品用0.04 mol/L NaOH提取,用弗罗里硅土柱净化。采用带紫外检测器的高效液相色谱仪测定,以乙腈与水为流动相梯度洗脱,在紫外波长229 nm下检测,用外标法定量。结果表明,5种除草剂在质量浓度0.05~5.00 mg/L的线性关系良好,相关系数(R)达0.999 7~0.999 9;土壤和糙米中添加水平为0.05~1.00 mg/kg时,5种除草剂的平均回收率为78.8%~107.8%,相对标准偏差(RSD≤7.5, n=5)为1.1%~9.2%;当水中添加水平为0.01~0.50 mg/L时,平均回收率为86.2%~109.2%,相对标准偏差(RSD≤6.5, n=5)为1.2%~6.5%。5种除草剂的检出限为0.01~0.02 mg/kg。方法在土壤、糙米和水样中的定量限分别为0.05、0.05 mg/kg和0.01 mg/L。该方法的前处理过程简单,且准确度、精密度和灵敏度均符合农药残留分析的技术要求。

    Abstract:

    To simultaneously determine residues of five herbicides, namely MCPA,2,4,5–T, haloxyfop–p–methyl, quizafop–p–ethyl and fluazifop–p–butyl in paddy soil, water and coarse rice, a new method was developed using high performance liquid chromatography . The residues in soil was extracted with mixed solution of 0.05% ortho-phosphoric acid and aetonitrile (volume ratio of 1∶2), and those in water was extracted with ethyl acetate , while in coarse rice was dissolved by 0.04 mol/L sodium hydroxide aqueous, then purified by a florisil column. Five herbicides were detected at uv wavelength of 229 nm with acetonitrile-water (pH=3) as mobile phase through gradient elution in HPLC, external standard was adopted as the quantification method. The linearity was good (r>0.999 7) in concentration range of 0.05 to 5.00 mg/L .Mean recoveries of five herbicides in soil and coarse rice were between 78.8% and 107.8% (RSD≤7.5, n=5) at fortification levels of 0.05 to 1.00 mg/kg, while they were between 86.2% and 109.2%(RSD≤6.5, n=5)in water at levels from 0.01 to 0.50 mg/kg. Under these optimal condition, The limit of detection for the five ingredients were between 0.01 to 0.02 mg/kg, and the limit of quantification in soil, coarse rice and water were 0.05 mg/kg, 0.05 mg/kg, and 0.01 mg/L respectively. Pre-treatment process of the method was simple, and sensitivity and accuracy of the method meet the technical requirement for the analysis and detection of pesticide residues.

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吴亮,龚道新,张小东,聂红英,杨丽华.高效液相色谱法同时检测稻田样品中5种除草剂的残留量[J].湖南农业大学学报:自然科学版,2016,42(3):.

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  • 在线发布日期: 2016-06-01
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