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采用带紫外检测器的高效液相色谱仪(HPLC-UV),建立了同时检测呋虫胺、吡虫啉和啶虫脒在稻田水、稻田土壤、水稻植株、稻秆、稻壳和糙米中残留量的检测方法。稻田水、稻田土壤、水稻植株、稻秆、稻壳样品用乙腈提取,糙米样品用V(乙腈)∶V(水)=1∶1混合溶液提取。稻田水无需净化,其余样品用弗罗里硅土柱净化。HPLC-UV测定,流动相为V(甲醇)∶V(水)=30∶70,流速采用梯度流速,紫外检测波长为254 nm。结果表明:在0.05~10 mg/L范围内,3种农药的质量浓度与其相对应的色谱峰面积之间呈良好的线性关系,线性方程分别为呋虫胺:y=62.55x+4.039 2(R2=0.999 2);吡虫啉:y=99.968x+7.525 1(R2=0.998 6);啶虫脒:y=97.084x+6.072(R2=0.999 4)。在0.05~2 mg/kg添加水平下,样品中呋虫胺、吡虫啉和啶虫脒的平均回收率在81%~99%之间,相对标准偏差(RSD,n=5)在1.2%~7.9%之间。该方法的前处理过程较简单,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。
The simultaneous determination of residues of dinotefuran, imidacloprid and acetamiprid in rice paddy soil, paddy soil, rice plants, rice straw, rice hulls and brown rice was established by HPLC-UV with UV detector. The detection method. Paddy water, paddy soil, rice plants, rice straw and rice husk samples were extracted with acetonitrile. Brown rice samples were extracted with a mixture of V (acetonitrile): V (water) = 1: 1. The paddy water does not need to be purified and the remaining sample is purified with Florisil columns. HPLC-UV, the mobile phase was V (methanol): V (water) = 30:70, the flow rate was gradient flow rate, UV detection wavelength was 254 nm. The results showed that there was a good linear relationship between the mass concentration of three pesticides and the corresponding chromatographic peak area in the range of 0.05-10 mg / L, the linear equations were respectively: dinotefuran: y = 62.55x + 4.039 2 ( R2 = 0.999 2); imidacloprid: y = 99.968x + 7.5251 (R2 = 0.998 6); acetamiprid: y = 97.084x + 6.072 (R2 = 0.999 4). The average recoveries of dinotefuran, imidacloprid and acetamiprid in the samples ranged from 81% to 99% at 0.05-2 mg / kg with relative standard deviations (RSD, n = 5) ranging from 1.2% to 7.9 %between. The method of pretreatment process is relatively simple, and the accuracy, precision and sensitivity are in line with the technical requirements of pesticide residue analysis.