高效液相色谱法测定毒氟磷原药及可湿性粉剂中有效成分含量  

Determination of Dufulin in TK and WP Formulation by HPLC

作　　者：佟盟露 丁玉玲 贾孙悦 马腾飞 周芹[1,3,4] 姜宜飞 Tong Menglu;Ding Yuling;Ma Tengfei;Jia Sunyue;Zhou Qin;Jiang Yifei(Modern Agriculture and the Ecological Environment Academy of Heilongjiang University,Harbin Heilongjiang 150080,China;School of Chemistry and Materials Science,Heilongjiang University,Harbin Heilongjiang 150080,China;Beet Quality Supervision,Inspection and Test Center Ministry of Agriculture and Rural Affairs,Harbin Heilongjiang 150080,China;Laboratory of Quality&Safety Risk Assessment for Sugar Crops Products,Ministry of Agriculture and Rural Affairs,Harbin Heilongjiang 150080,China;Institute for the Control of Agrochemicals,Ministry of Agriculture and Rural Affairs,Beijing 100125,China)

机构地区：[1]黑龙江大学现代农业与生态环境学院,黑龙江哈尔滨150080 [2]黑龙江大学化学化工与材料学院,黑龙江哈尔滨150080 [3]农业农村部甜菜品质监督检验测试中心,黑龙江哈尔滨150080 [4]农业农村部糖料产品质量安全风险评估实验室,黑龙江哈尔滨150080 [5]农业农村部农药检定所,北京100125

出　　处：《农药科学与管理》2022年第9期36-45,共10页Pesticide Science and Administration

基　　金：《农药产品中有效成分测定通用分析方法-液相色谱法》体系建设“啶磺草胺等10个农药品种液相色谱分析方法建立”(14192195);现代农业产业技术体系建设项目“质量安全与营养品质评价”(CARS-170503)。

摘　　要：建立了在同一液相色谱条件下,毒氟磷原药及可湿性粉剂中有效成分含量的通用分析方法。试样用甲醇溶解,以甲醇-水为流动相(体积比为80:20),流速1.0mL/min,进样体积5.0μL,采用C色谱柱和二极管阵列检测器,反相高效液相色谱法,在波长270nm条件下对试样中的毒氟磷进行高效液相色谱分离,外标法定量,同时利用二极管阵列检测器进行了峰纯度检验,并且进行了不同实验室间的比对实验。结果表明,当毒氟磷质量浓度在101.6~1006.4mg/L之间时,与相应的峰面积呈现良好的线性关系,相关系数R~2为0.9998;可湿性粉剂中毒氟磷添加回收率为99.43%;原药及可湿性粉剂测定结果的相对标准偏差(RSD)分别为1.23%、1.61%,不同实验室不同仪器之间的重复性标准偏差(RSD)分别为0.5627%和0.5573%,再现性相对标准偏差(RSD)分别为0.7339%、0.8162%。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,适用于毒氟磷原药及可湿性粉剂中毒氟磷含量的测定。The purpose of this experiment is to establish a method for the determination of dufulin in technical(TC)and wettable powder(WP)under the same high performance liquid chromatography(HPLC)condition,with the mobile phase of methanol-water(80:20 v/v),flow rate of 1.0 mL/min and injection volume of 5.0μL.The samples were dissolved in methanol and separated on RP-HPLC with Ccolumn and diode array detector(DAD)at 270 nm and quantified using external standard method.The peak purity was checked through DAD detector and the method was validated in different laboratories.The results showed that good linearities corresponding to the peak area were obtained,with the correlation coefficient(R~2)of 0.9998.at the concentration ranged from 101.6 mg/L to 1006.4 mg/L.The recovery of dufulin in WP was found to be 99.43%;the RSD of TC and WP was 1.23%and 1.61%respectively.The values of RSDof different laboratories were 0.5627%and 0.5573%.The values of RSDwere 0.7339%and 0.8162%,respectively.The precision,accuracy and peak purity complies with the requirements of pesticide products analysis.The method is suitable for the determination of dufulin in technical and wettable powder.

关 键 词：毒氟磷 原药 可湿性粉剂 高效液相色谱 有效成分 

分 类 号：S482.2[农业科学—农药学] O657.72[农业科学—植物保护]