一种测定农药氨基寡糖素含量的高效液相色谱方法

A method for the determination of amino-oligosaccharin by high performance liquid chromatography

建立一种高效液相色谱法测定氨基寡糖素产品中有效成分含量的方法。用8 mol/L的盐酸在98℃下水解氨基寡糖素4 h,再以1-苯基-3-甲基-5-吡唑啉酮(PMP)为衍生剂对水解产物进行衍生,采用高效液相色谱法,以乙腈-磷酸盐缓冲液作为流动相,使用SB-C_(18)色谱柱和PDA检测器,在波长为254 nm下对氨基寡糖素母药及氨基寡糖素可溶液剂中氨基寡糖素的含量进行分析。该方法的氨基寡糖素线性范围为1~264mg/L,线性相关系数为0.9999,氨基寡糖素母药及氨基寡糖素可溶液剂的相对标准偏差分别为0.69%和1.43%,水解回收率分别为95.1%~98.2%和95.2%~99.4%,衍生回收率分别为97.6%~104.1%和98.5%~103.8%。该方法准确、快速,适用于氨基寡糖素相关产品中有效成分的检测。

A high performance liquid chromatography method was established for the determination of amino-oligosaccharin.Amino-oligosaccharin was first hydrolyzed into glucosamine by 8 mol/L hydrochloric acid at 98℃ for 4 h,and then glucosamine derived with 1-phenyl-3-methyl-5-pyrazolone(PMP).The chromatographic separation of the above derivations was carried out on an Agilent SB-C_(18) column using acetonitrile-phosphate buffer as the mobile phase at 254 nm.The linearity range of this method was 1-264 mg/L,and the linear correlation coefficient was 0.9999.The relative standard deviations of amino-oligosaccharin TK and SL were 0.69% and 1.43%,the hydrolysis recoveries were 95.1%-98.2% and 95.2%-99.4%,and the derivatization recoveries were 97.6%-104.1% and 98.5%-103.8%,respectively.The method is accurate and rapid,and suitable for the detection of amino-oligosaccharin.