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    附蒸发光散射检测器的高效液相色谱法测定水溶性肥料中3种季铵盐类植物生长调节剂的含量

    Determination of 3 Quaternary Ammonium Salt Plant Growth Regulators in Water-Soluble Fertilizer by High Performance Liquid Chromatography with Evaporation Light Scattering Detector

    • 摘要: 取1.0 g水溶性肥料样品,加入80 mL水,超声溶解10 min,用水定容至100 mL,过0.22 μm滤膜。在CNWSIL SCX COLUMN强阳离子交换色谱柱上用体积比为90:10的0.4%(体积分数)三乙胺溶液(乙酸调节pH至6.0)和乙腈的混合溶液分离滤液中的氯化胆碱、矮壮素、甲哌鎓等3种季铵盐类植物生长调节剂。分离得到的目标化合物用蒸发光散射检测器检测,设置蒸发温度和雾化温度均为80℃,雾化器流量为1.8 L·min-1,增益值为8。结果显示,3种目标化合物可在13 min内完全分离,其质量浓度的对数值与其对应的峰面积的对数值均在20~200 mg·L-1内呈线性关系,检出限(3S/N)均为4 mg·L-1;对空白样品进行加标回收试验,回收率为95.9%~105%,测定值的相对标准偏差(n=6)为1.2%~2.8%。方法用于实际样品的分析,氯化胆碱、矮壮素、甲哌鎓均在一定程度上检出。

       

      Abstract: 1.0 g of the water-soluble fertilizer sample was taken, and 80 mL of water was added. The mixture was dissolved ultrasonically for 10 min, and the obtained solution was made its volume up to 100 mL and then filtered through 0.22 μm filtration membrane. A mixture of 0.4% (φ) triethylamine solution (adjusting pH to 6.0 with acetic acid) and acetonitrile in the volume ratio of 90:10 was used to separate 3 quaternary ammonium salt plant growth regulators, including choline chloride, chlormequat and mepiquat chloride, from the filtrate on CNWSIL SCX COLUMN. The separated target compounds were detected by evaporation light scattering detector. The evaporation temperature and atomization temperature were set to 80℃, atomization gas flow was 1.8 L·min-1, and gain value was 8. As shown by the results, linear relationships between the log values of mass concentration and corresponding peak area of 3 quaternary ammonium salt plant growth regulators were found in the same range of 20-200 mg·L-1, with the same detection limits (3S/N) of 4 mg·L-1. Recovery test was carried out with blank samples, giving results in the range of 95.9%-105%, with RSDs (n=6) of the determined values in the range of 1.2%-2.8%. The method was applied for the analysis of actual samples, and choline chloride, chlormequat and mepiquat chloride were all detected to a certain extent.

       

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