高效液相色谱法测定啶菌唑(口恶)原药及乳油中有效成分含量

Active ingredients in pyrisoxazole technical and emulsifiable concentrate: determination by HPLC

[目的]为了建立在同一液相色谱条件下啶菌(口恶)唑原药及乳油中有效成分含量的通用分析方法。[方法]样品用甲醇溶解,采用反相高效液相色谱法,流动相为甲醇-水溶液(体积比78∶22),流速1.0 mL/min,进样量5μL,使用Symmetry-C18色谱柱和二极管阵列检测器,在波长220 nm下对试样中的啶菌(口恶)唑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协同验证。[结果]方法的线性范围在102.5~1024.2 mg/L之间,线性相关系数R2为0.9999;啶菌(口恶)唑原药和乳油测定结果的相对标准偏差(RSD)值分别为1.00%、1.07%;乳油的添加回收率平均值为100.68%;多个实验室间协同验证的重复性相对标准偏差(RSDr)原药及乳油分别为0.3662%、0.8538%,再现性相对标准偏差(RSDR)分别为0.4771%、1.0590%。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,适用于啶菌(口恶)唑原药及乳油中啶菌(口恶)唑含量的测定。

[Aims] This study aims to establish a general method for the determination of the active ingredient in pyrisoxazole technical(TC) and the emulsifiable concentrate(EC) under the same high performance liquid chromatography(HPLC) condition. [Methods] The samples were dissolved in methanol, and analyzed by RP-HPLC.The mobile phase was methanol-water(78∶22, by vol), the flow rate was 1.0 mL/min and the amount of injection was5 μL. The samples were separated on the Symmetry-C18 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. [Results] The result showed good linearity in the concentration ranged from 102.5 to 1024.2 mg/L, with the correlation coefficient(R2) of 0.9999. The RSD of measurement results were 1.00% and 1.07% respectively. The recovery of EC was 100.68%. RSDr of different laboratories were 0.3662%and 0.8538% respectively. RSDR were 0.4771% and 1.0590% respectively. The precision, accuracy and peak purity results meet the requirements of analysis for pesticide products. The method is suitable for the determination of active ingredient for pyrisoxazole in technical and emulsifiable concentrate.