超高效液相色谱法测定噁草酸原药及乳油中有效成分含量

Determination of active ingredient for propaquizafopin in technical material and emulsifiable concentrate by UPLC

建立了在同一液相色谱条件下噁草酸原药及乳油中有效成分含量的测定方法。样品以甲醇溶解,使用C_(18)色谱柱和二极管阵列检测器,甲醇-水溶液(体积比80∶20)为流动相,等度洗脱,在波长235 nm下外标法定量。使用二极管阵列检测器对色谱峰纯度进行了检验,并进行了方法验证。结果表明:方法为100.5~1003.9 mg·L^(-1)线性范围内线性关系良好,相关系数R^(2)为0.9995;原药及乳油的添加回收率分别为100.78%、100.44%;标准偏差为0.35%、0.02%,变异系数(RSD)分别为0.21%、0.39%;不同实验室间重复性相对标准偏差分别为0.2096%、1.5595%,再现性相对标准偏差分别为0.4540%、2.0344%。该方法的技术指标均符合农药产品分析方法的要求,适用于噁草酸原药及乳油中噁草酸含量的测定。

A analytical method was established to determine active ingredient of propaquizafop in technical material(TC)and emulsifiable concentrate(EC)using the same ultra-high performance liquid chromatography(UPLC)condition.The samples were dissolved in methanal and the mixture of methanol and water(80∶20)was applied as the mobile phase.The separation was achieved by using C_(18) column,isocratic elution and diode array detector(DAD)at 235 nm.The quantitative result was calculated by external standard method.In addition,the peak purity was checked by DAD.The nalytical method was futher confirmed by three different laboratories.The results showed good linearities in the concentration range of 100.5~1003.9 mg·L^(-1),with the correlation coefficients(R^(2))of 0.9995.The recoveries of TC and EC were 100.78%and 100.44%,respectively.RSD were 0.21%and 0.39%.RSD of different laboratories were 0.2096%and 1.5595%,RSDr were 0.4540%and 2.0344%,respectively.The results of precision,accuracy and peak purity meet the requirements of analysis for pesticide products.It is suitable for the determination active ingredient for propaquizafopin in technical material and emulsifiable concentrate.