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对确立的以甲醇为分散萃取溶剂,乙二胺-N-丙基硅烷(PSA)、十八烷基硅烷键合相(C18)和石墨化碳黑(GCB)为基质分散材料的大豆植株、籽粒及豆田土壤咪唑乙烟酸残留基质分散萃取前处理方法,进行了乙腈等度洗脱的高效液相色谱(HPLC)残留样品外标定量方法条件的优化。结果表明:优化色谱条件下,咪唑乙烟酸的色谱保留时间为6.97 min,在0.01~10.0 mg·L-1质量分数范围内与对应色谱峰积分面积线性响应良好,回归方程为y=4.003 8 x-0.275 6(R2=0.999 5),回收率均在85%以上,相对标准偏差均小于9%;该色谱条件下仪器检出限为0.104 ng,方法的最低检测浓度分别为0.024(植株),0.033(籽粒)和0.026 mg·kg-1(豆田土壤),表明该残留样本前处理方法和样品检测方法简便、高效、经济、可靠,可满足咪唑乙烟在大豆植株、大豆籽粒及豆田土壤中残留定量检测要求。
For the established soybean plants with methanol as disperse extraction solvent, ethylenediamine-N-propylsilane (PSA), octadecylsilane-bonded phase (C18) and graphitized carbon black (GCB) The pretreatment methods of disperse extraction of imazethapyr residues in kernels and soils in grain and soybean fields were optimized for the external standard quantitation of residual samples by high performance liquid chromatography with isocratic elution of acetonitrile. The results showed that under optimized chromatographic conditions, the retention time of imazethapyr was 6.97 min, and the linear regression equation was y = 4.003 8 x-0.275 in the range of 0.01-10.0 mg · L-1. (R2 = 0.999 5). The recoveries of the two methods were over 85% and the relative standard deviations (RSDs) were both less than 9%. The detection limit was 0.104 ng under the chromatographic conditions. The minimum detectable concentrations were 0.024 Grain) and 0.026 mg · kg-1 (soybean soil), indicating that the residual sample pretreatment method and sample detection method are simple, efficient, economical and reliable, and can meet the quantitative determination of residues of imazethapyr in soybean plants, soybean seeds and soya bean soils Testing requirements.