柱前衍生-液相色谱法测定草铵膦中间体3-(甲基烷氧膦酰基)丙醛

Determination of 3-(Methylalkyloxylphosphonyl)propionaldehyde by Pre-column Derivatization Coupled with HPLC

建立柱前衍生-液相色谱法测定合成的草铵膦关键中间体3-(甲基烷氧膦酰基)丙醛的含量的方法。3-(甲基烷氧膦酰基)丙醛在60℃与2,4-二硝基苯肼(DNPH)衍生反应20 min后,在色谱柱:CLCODS C_(18)(150 mm×6.0 mm×5μm),流速:1.0 m L/min,检测波长:360 nm,流动相:v(甲醇)∶v(乙腈)∶v(水)=27.5∶27.5∶45.0的条件下进行测定,外标法定量。结果表明:该分析方法在0.03~0.30 g/L浓度范围内线性关系良好,加标回收率保持在98.0%~99.3%之间。

A method for determination of 3-（methylalkyloxylphosphonyl） propionaldehyde, a key intermediate for glufosinate ammonium was established by the pre-column derivatization coupled with HPLC. The 3- （methylalkyloxylphosphonyl） propionaldehyde was derivatized using 2,4-Dinitrophenylhydrazine （DNPH） for 20 minutes at 60℃, then separated on the chromatographic column of CLC-ODS C18 （150 min×6.0 mm×5 μm）. The separation conditiona were set as foUowings： the flow rate was 1.0 mL/min; the detection wavelength was 360 nm; the mobile phase was consisted of methanol, acetonitrile and water （27.5 ： 27.5 ： 45.0）. The results showed that the linear relationship was good in the range of 0.03-0.30 g/L and the recovery rates were 98.0%-99.3%.