高效液相色谱法同时测定农药产品中溴敌隆和溴鼠灵顺反异构体

Simultaneous determination of cis and trans isomers of bromadiolone and brodifacoum in pesticide products by HPLC

采用高效液相色谱仪建立了一种同时测定农药产品中溴敌隆和溴鼠灵顺反异构体的方法,旨在为该产品的质量控制提供技术支撑。该方法确定的色谱条件:检测器为二极管阵列检测器;流动相A为乙腈,B为pH=3的磷酸水溶液,梯度洗脱程序:A为60%时保持20 min,20.1 min后A由60%升至80%时保持10 min,25.1 min后A由80%降至60%。检测波长为265 nm(0~16 min)和254 nm(16.1~30 min),采用外标法定量。结果表明,在125~12500 mg/kg的质量浓度范围内,农药质量浓度与其响应值之间呈现出良好的线性相关;添加浓度为125、1250、12500 mg/kg时,溴敌隆A、溴敌隆B、溴鼠灵A和溴鼠灵B的平均加标回收率为93%~106%,相对标准偏差为0.41%~2.6%,能够满足检测要求。本方法可用于农药产品中顺反异构体溴敌隆和顺反异构体溴鼠灵的检测工作。

The study aims to establish a analysis method by HPLC with DAD detector for simultaneous determination of cis and trans isomers of bromadiolone and bromadiolone in pesticide products.The external standard quantitative method used in this paper can provide technical support for the quality control of the products.The chromatographic conditions were as follows:the detector was DAD;mobile phase A was acetonitrile;B was phosphoric acid solution(pH=3);gradient elution procedure:hold for 20 min when A was 60%,A was 80%after 20.1 min and hold for 10 min,A was 60%after 25.1 min.The detection wavelength was 265 nm(0-16 min)and 254 nm(16.1-30 min).The detection results showed a good linearity between the concentration and its response value in the concentration range of 125-12500 mg/kg.The average recovery of bromadiolone A,bromadiolone B,brodifaconazole A and brodifaconazole B was between 93%and 106%and the relative standard deviations was between 0.41%and 2.6%at the added concentrations of 125,1250 and 12500 mg/kg,which can meet the detection requirements.This method can be used for the determination of cis and trans isomers of bromadiolone and brodifacoum in pesticide products.