高效液相色谱法测定啶氧菌酯悬浮剂及水分散粒剂中有效成分含量

Active Ingredients in Picoxystrobin Suspension Concentrate and Water Dispersible Granule:Determination by HPLC

为了建立在同一液相色谱条件下啶氧菌酯悬浮剂及水分散粒剂中有效成分含量的通用分析方法,样品用乙腈溶解,采用反相高效液相色谱法,流动相为乙腈-水溶液(体积比80:20),流速1.0 m L/min,进样量5μL,使用Symmetry-C_(18)色谱柱和二极管阵列检测器,在波长220 nm下对试样中的啶氧菌酯进行高效液相色谱分离,外标法定量。此外,利用二极管阵列检测器进行了峰纯度检验及不同实验室方法验证。结果表明:方法的线性范围在100.1~1000.8 mg/L之间,线性相关系数R^(2)为0.9993;悬浮剂及水分散粒剂的添加回收率平均值分别为100.64%、99.74%,测定结果的相对标准偏差(RSD)值分别为1.31%、0.69%;不同实验室不同仪器之间的重复性标准偏差悬浮剂及水分散粒剂分别为0.8052%、0.6003%,再现性相对标准偏差(RSD_(R))分别为0.8560%、1.5625%。方法精密度、准确度及峰纯度结果均符合农药产品分析方法的要求,适用于啶氧菌酯悬浮剂及水分散粒剂中啶氧菌酯含量的测定。

In order to establish a general method to determine active ingredient in picoxystrobin suspension concentrate(SC)and water dispersible granule(WG)using the same high performance liquid chromatography(HPLC)condition,the samples were dissolved with acetonitrile,and analyzed by RP-HPLC.The mobile phase was acetonitrile-water(volume ratio 80:20),the flow rate was 1.0 m L/min and the amount of injection was 5.0μL.Separation was achieved on the Symmetry-C_(18)column and diode array detector(DAD)at 220 nm,and the quantitative result was calculated by external standard method.In addition,the peak purity was checked through DAD and the method was tested by different laboratories.The result showed good linearities in the concentration ranged from 100.1 mg/L to 1000.8 mg/L,with the correlation coefficient(R^(2))of 0.9993.The recovery of SC and WG were 100.64%and 99.74%,respectively.The RSD of measurement results were 1.31%and 0.69%respectively.RSD of different laboratories were 0.8052%and 0.6003%.RSD_(R)were 0.8560%and1.5625%,respectively.The precision,accuracy and peak purity results meet the requirements of analysis for pesticide products.The method is suitable for the determination active ingredient for picoxystrobin in suspension concentrate and water dispersible granule.