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[目的]建立水稻植株和糙米样品中异稻瘟净的残留分析方法。[方法]植株和糙米用丙酮和乙酸乙酯混合溶剂提取,采用SPE C18柱和SPE NH2柱二维净化,气相色谱火焰热离子检测器(FTD)测定。[结果]在0.005~5.0 mg/kg的浓度范围内,异稻瘟净的浓度与峰面积成良好线性关系(r=0.999 8)。在添加浓度分别为0.01、0.1、1.0 mg/kg时,水稻植株中的添加回收率为72.6%~99.7%,相对标准偏差为5.65%~8.48%;糙米中的添加回收率为81.6%~97.6%,相对标准偏差为3.74%~7.63%。异稻瘟净的最低检出量为5×10-12g;水稻植株和糙米最小检出浓度分别为2和0.5μg/kg。[结论]该方法检测限低,灵敏度高、重现性好、可操作性强,满足农业部农药残留试验准则要求(NY788-2004)。
[Objective] The research aimed to establish a method for the analysis of the residues of different rice blast in rice and brown rice samples. [Method] The plants and brown rice were extracted with a mixture of acetone and ethyl acetate. The two phases were purified by SPE C18 column and SPE NH2 column and analyzed by gas chromatography flame ionization detector (FTD). [Result] In the concentration range of 0.005-5.0 mg / kg, the net concentration of iso-blast was linear with the peak area (r = 0.999 8). The recoveries of rice plants were 72.6% -99.7% with relative standard deviations of 5.65% -8.48% at the concentration of 0.01, 0.1 and 1.0 mg / kg, respectively. The recoveries of brown rice were 81.6% -97.6 %, The relative standard deviation is 3.74% ~ 7.63%. The detection limit of the isolates of rice blast was 5 × 10-12g. The minimum detectable concentrations of rice plants and brown rice were 2 and 0.5μg / kg, respectively. [Conclusion] This method has the advantages of low detection limit, high sensitivity, good reproducibility, strong maneuverability and meeting the requirements of the Ministry of Agriculture Pesticide Residue Test (NY788-2004).