24%螺螨双酯悬浮剂中有效成分及相关杂质的高效液相色谱分析

Determination of spirobudiclofen and related impurity in spirobudiclofen 24%SC by HPLC

[目的]建立了一种对24%螺螨双酯混悬剂中螺螨双酯及相关杂质3-(2,4-二氯苯基)-4-羟基-1-氧杂螺[4.5]癸-3-烯-2-酮(BAJ-2510)含量测定的高效液相色谱分析方法。[方法]以0.1%磷酸水溶液和乙腈作为流动相,梯度洗脱,使用Ultimate XB-C_(18)色谱柱和PDA检测器,在245 nm波长下对悬浮剂中的螺螨双酯和BAJ-2510进行分离和含量分析。[结果]螺螨双酯和BAJ-2510线性相关系数分别为0.9999和0.9998,标准偏差分别为0.001和0.000 05,变异系数RSD分别为0.41%和0.38%,平均回收率分别为100.9%和101.7%。[结论]该方法操作简便,精密度好,准确度高,线性关系良好,为该悬浮剂的市场监管和生产企业的质量检测及控制提供了可靠的检测方法。

[Aims]This study aims to establish a HPLC method for quantitative analysis of spirobudiclofen and 3-(2,4-dichlorophenyl)-4-hydroxy-1-oxaspiro[4.5]dec-3-en-2-one(BAJ-2510)in spirobudiclofen 24%SC.[Methods]Spirobudiclofen and related impurity BAJ-2510 in the sample were separated and determined with the mixture of o.1%phosphotous acid aqueous solution and acetonitrile as mobile phase with Ultimate XB-C_(18) column and PDA detector at 245 nm,and quantified by external standard method.[Results]The linear correlation coefficients of spirobudiclofen and BAJ-2510 were 0.9999 and 0.9998,the standard deviation were 0.001 and 0.00005,the coefficient of variation were 0.41%and 0.38%,and the average recoveries were 100.9%and 101.7%,respectively.[Conclusions]The method is easy to operate,with high precision,high accuracy and good linear relationship,which provides a reliable detection method for the market supervision of spirobudiclofen 24%SC and the quality detection and control of the production enterprises.