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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 the determination of 3- (methylalkoxyphosphino) propionaldehyde, a key intermediate of synthetic phosphinothricin, was established by pre-column derivatization-liquid chromatography. After the reaction of 3- (methylalkoxy phosphoryl) propanal with DNPH at 60 ℃ for 20 min, the reaction was carried out on a chromatographic column: CLCODS C 18 (150 mm × 6.0 mm × 5μm), flow rate: 1.0 m L / min, detection wavelength: 360 nm, mobile phase v: methanol: v acetonitrile: v water 27.5:27.5:45.0, . The results showed that the linearity of the method was good in the concentration range of 0.03-0.30 g / L, and the recoveries of spiked samples kept between 98.0% and 99.3%.