HPLC法分离测定一种嘧啶胺类新农药

[目的]采用HPLC法对一种嘧啶胺类新农药进行分离测定研究。[方法]对HPLC的最佳检测波长、流动相进行筛选,并对2-甲硫基-4-氨基-5-嘧啶甲醛和2-甲硫基-4-氨基-5-嘧啶甲醇的进行线性关系考察。在此基础上对样品进行测定并检测其精确度。[结果]试验确定最佳紫外吸收波长为251 nm,以此为检测波长,采用反相ODS-C18色谱柱,确定以甲醇∶水=70∶30(V/V,%)为流动相;检测出2-甲硫基-4-氨基-5-嘧啶甲醛和2-甲硫基-4-氨基-5-嘧啶甲醇样品线性范围为0.001～0.100 mg/ml;得到2-甲硫基-4-氨基-5-嘧啶甲醛的RSD为0.67%,2-甲硫基-4-氨基-5-嘧啶甲醇的RSD为0.85%。[结论]该方法可同时分离测定嘧啶胺类新农药2-甲硫基-4-氨基-5-嘧啶甲醛及其中间体2-甲硫基-4-氨基-5-嘧啶甲醇,且方法快速、准确。

The Separation of a New Pyrimidine Pesticide by HPLC

[Objective]The aim was to study the separation and determination of a new pyrimidine pesticide by HPLC.[Method]The best detected wavelength and mobile phase of HPLC were screened,moreover,the linear relation between 2-methylthio-4-amino-5-pyrimidine methanol and 2-methylthio-4-amino-5-pyrimidine formaldehyde was investigated.Based on this,the samples were determined and their precisions were detected.[Result] Based on the test,the best ultraviolet absorption wavelength was 251 nm,and it was viewed as detected wavelength;using opposite phase ODS-C18 chromatographic column,it determined that carbinol∶water=70∶30(V/V,%) was mobile phase,and the samples’ linear range of 2-methylthio-4-amino-5-pyrimidine methanol and 2-methylthio-4-amino-5-pyrimidine formaldehyde was 0.001-0.100 mg/ml;RSD of 2-methylthio-4-amino-5-pyrimidine methanol was 0.67%,RSD of 2-methylthio-4-amino-5-pyrimidine formaldehyde was 0.85%.[Conclusion]The method can separate and determine new pyrimidine pesticide:2-methylthio-4-amino-5-pyrimidine formaldehyde and its midbody:2-methylthio-4-amino-5-pyrimidine methanol simultaneously,and the method is rapid and accurate.