嗪草酮中间体——三甲基丙酮酸高效液相色谱定量分析

建立一种采用高效液相色谱法定量分析除草剂嗪草酮的重要中间体三甲基丙酮酸的方法,为嗪草酮的高效合成提供有效保证。选用Agilent ZORBAX SB-Aq色谱柱、紫外检测器,以乙腈和水(0.01 mol/L KH_2PO_4)(体积比15:85)为流动相,流速1.0 mL/min,柱温为室温,波长215 nm定量分析三甲基丙酮酸。三甲基丙酮酸的色谱保留时间为4.8 min,线性相关系数为0.999 9,方法的标准偏差为0.081,变异系数为0.17%,平均回收率为99.75%。此方法分析快速、简便、分离完全、结果重现性好,所得结果可信度高,是一种实用的中间控制分析方法。

Quantitative Analysis Method of 3,3-Dimethyl-2-oxobutyric Acid by HPLC

A HPLC method for quantitative of 3,3-dimethyl-2-oxobutyric acid has been established. 3,3-Dimethyl-2-oxobutyric acid was tested by HPLC with Agilent ZORBAX SB-Aqcolumn at 215 nm, and acetonitrile/ water（0.01mol/L KH2PO4）（15：85, by vol） was used as the mobile phase with flow rate of 1.0 mL/min. The results showed that under the optimal conditions, the retention time for 3,3-dimethyl-2-oxobutyric acid was 4.8 min, the linear correlation coefficient was 0.9999, the standard deviations was 0.081, the coefficient of variation was 0.17%, the average recovery was 99.75%. The method is simple, rapid, and shows high credibility data immediately, which is a useful analysis method for intermediate control.