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建立化学杂交剂SQ-1在谷子叶片和小穗中残留检测的高效液相色谱法,并研究其在谷子叶片和小穗中的消解动态。样品经乙腈提取,N-丙基乙二胺净化,外标法定量。该检测方法在1~1 000 mg/L范围内,化学杂交剂SQ-1质量浓度与色谱峰面积呈良好的线性关系,线性方程为y=30 377x+27 634,相关系数为0.999 9,最低检出限为0.05 mg/kg。在10~500 mg/kg添加范围内,化学杂交剂SQ-1在谷子叶片和小穗中的平均回收率为87.0%~95.5%,相对标准偏差为0.74%~2.28%。结果表明:化学杂交剂SQ-1可以从谷子叶片运输到小穗中,在小穗中的动态变化呈现出“先升高后降低”的趋势。其在谷子叶片中的半衰期为1.83~2.08 d,在喷施21 d后叶片中几乎检测不到化学杂交剂SQ-1残留,而在小穗中的半衰期为25.21~28.41 d,其消解速度明显慢于叶片中的消解速度。
A high performance liquid chromatography (HPLC) method was developed for the determination of chemical hybridization agent SQ-1 in millet leaves and spikelets. The digestion dynamics in millet leaves and spikelets were also studied. Samples were extracted with acetonitrile, N-propyl ethylenediamine purification, external standard method. The detection method was in the range of 1 ~ 1 000 mg / L, and the chemical hybridization reagent SQ-1 had a good linear relationship with the chromatographic peak area. The linear equation was y = 30 377x + 27 634, the correlation coefficient was 0.999 9, The detection limit is 0.05 mg / kg. In the range of 10 ~ 500 mg / kg, the average recoveries of chemical hybridization agent SQ-1 in millet leaves and spikelets were 87.0% -95.5% with relative standard deviations of 0.74% -2.28%. The results showed that the chemical hybridization agent SQ-1 could be transported from spikelets of millet to spikelets, and the dynamic changes in spikelets showed the tendency of “increasing first and then decreasing”. Its half-life in the leaves of millet was 1.83 ~ 2.08 d. After spraying for 21 d, almost no detectable chemical hybridization agent SQ-1 remained in the leaves, while the spikelet had a half-life of 25.21-28.41 d, showing a significant digestion rate Slower than digestion speed in leaves.