摘要
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.
作者
马腾飞
贾孙悦
刘琳
周芹
高金胜
Ma Tengfei;Jia Sunyue;Liu Lin;Zhou Qin;Gao Jinsheng(Modern Agriculure and the Ecological Enwironment Academy of Heilongiang Univrity,Harbin 150080;School of Chemistry and Marerials Science,Heilongjiang University,Harbin 150080;Beet Quality Supervision,Inspection and Test Center Ministry of Agriculture and Rural Affairs,Harbin 150080;Laboratory of Quality&Safety Risk Asessnent for Sugar Crops Products,Ministry of Agriculture and Rural Affairs,Harbin 150080)
出处
《中国农学通报》
2021年第27期117-124,共8页
Chinese Agricultural Science Bulletin
基金
国家甜菜现代农业产业技术体系项目“质量安全与营养品质评价”(CARS-170503)《
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)。
关键词
啶氧菌酯
悬浮剂
水分散粒剂
高效液相色谱
有效成分
picoxystrobin
suspension concentrate
water dispersible granule
HPLC
active ingredient