丙硫菌唑和肟菌酯混剂产品高效液相色谱分析方法

Analysis prothionazole·trifloxystrobin mixture by HPLC

建立一种可以同时检测丙硫菌唑和肟菌酯混剂中2种有效成分的高效液相色谱法,为产品质量控制提供技术支持。以甲醇-0.1%磷酸水溶液(体积比70∶30)为流动相,采用流动相溶解试样,选取XDB-C_(18)为填充物的不锈钢色谱柱和紫外检测器,在254 nm紫外波长下,对样品中丙硫菌唑和肟菌唑进行分离和定量分析。采用HPLC-DAD峰纯度分析法鉴别丙硫菌唑和肟菌酯杂质干扰程度,主要成分的最小峰纯度相似度均为1.0000,最小峰纯度阈值均为0.9999,最小峰纯度指数均为0,无干扰成分。结果表明,该方法测得丙硫菌唑的保留时间为17.8 min,线性相关系数为0.9997,标准偏差为0.02,变异系数为0.2%,平均回收率为99.6%;肟菌酯的保留时间为26.1 min,线性相关系数为0.9999,标准偏差为0.02,变异系数为0.2%,平均回收率为100.9%。且经制剂空白验证无非分析物干扰。该方法操作简便,快速稳定,结果准确,可满足混剂中丙硫菌唑和肟菌酯定量分析的要求。

A HPLC method was established to separate and quantitatively analyse the content of active ingredients prothionazole and trifloxystrobin in the formulation in order to provide the support for the quality control for the product.Using the mixture solution of acetonitrile and 0.1%(wt%)phosphoric acid solution(70∶30,by vol)as the mobile phase,Prothionazole and trifloxystrobin were dissolved by the mobile phase,and were separated on XDB-C18 stainless steel column,and analysed at 254 nm UV-absobance detertor wavelength.HPLC-DAD peak purity was used to identify the degree of impurity interference with prothionazole and trifloxystrobin.The minimum peak purity similarity of both active ingredients was 1.0000,the minimum peak purity threshold was 0.9999,and the minimum peak purity indexe was 0,showing no interfering components.The results showed that the retention time of prothionazole was 17.8 min and the linear correlation coefficient was 0.9997,the standard deviation was 0.02,the variation coefficient was 0.2%,and average recovery was 99.6%.The retention time of prothionazole was 26.1 min,the linear correlation coefficient was 0.9999,the standard deviation was 0.02,the variation coefficient was 0.2%,and average recovery was 100.9%.There was no nontarget interfering substances existing which was validated by the blank formulation.The method is simple,rapid,stable and easy to operate,which is suitable for quantitative analysis of prothionazole and trifloxystrobin in the mixture.