离子对反相高效液相色谱-蒸发光散射检测法测定三乙膦酸铝的含量

Determination of fosetyl-aluminium by ion-pair reversed phase-high performance liquid chromatography with evaporative light scattering detection

建立了以正丁胺为离子对试剂的反相高效液相色谱分析三乙膦酸铝含量的方法。采用Symmetry ShieldRP18色谱柱分离,以甲醇-0.5%正丁胺水溶液(冰乙酸调节pH5.0)(体积比为8∶92)为流动相,流速为0.8mL/min,蒸发光散射检测器(ELSD)检测。在上述条件下,三乙膦酸铝与其主要杂质亚磷酸盐、硫酸盐可以获得分离。在100～1 200mg/L范围内,进样质量与峰面积的双对数值呈良好的线性关系。100mg/L和1 000mg/L两种质量浓度添加水平的回收率分别为100.58%和99.53%,其相对标准偏差(RSD)分别为0.62%和0.49%。该方法简便快捷,为三乙膦酸铝的定量分析提供了更加有效可靠的方法。

Ion-pair reversed phase-high performance liquid chromatography （RP-HPLC） with evaporative light scattering detection （ ELSD ） has been established for the analysis of fosetylaluminium and relevant impurities in technical or formulated substance. The method was achieved on a Symmetry Shield RP18 column by using n-butylamine as ion-pairing agent. The mobile phase was methanol-redistilled water containing 0.5% n-butylamine which was adjusted pH 5.0 with acetic acid （8： 92, v/v） and the flow rate was set at 0. 8 mL/min. The active ingredient fosetyl-aluminium was successfully separated from relevant impurities under the conditions. The calibration curve was linear in the range of 100 - 1 200 mg/L. The average recoveries of two fortification levels （ 100 mg/L and 1 000 mg/L） were 100.58% and 99.53%, and the relative standard deviations （RSDs） were 0.62% and 0.49%, respectively. The method is rapid, simple and accurate which provides another new and reliable means for the analysis of fosetylaluminium in its technical or formulated substance.