多菌灵、苯菌灵、甲基硫菌灵原药中2-羟基-3-氨基吩嗪(HAP)和2,3-二氨基吩嗪(DAP)有害杂质的分析方法

Determination Method of 2-Hydroxy-3-aminophenazine(HAP) and2,3-Diaminophenazine(DAP) in Carbendazim,Benomyl and Thiophanate-methyl Technical by HPLC

[目的]利用高效液相色谱法对多菌灵、苯菌灵、甲基硫菌灵原药中的有害杂质2-羟基-3-氨基吩嗪（HAP）和2,3-二氨基吩嗪（DAP）进行分析。建立测定HAP和DAP的液相色谱的检测方法。[方法]色谱条件：Hypersil ODS不锈钢色谱柱,使用pH值8.0磷酸二氢钾的水缓冲溶液和甲醇作为流动相,紫外检测器检测波长453 nm,对各原药产品中的HAP和DAP有害杂质进行定量分析。[结果]方法中HAP的回收率为89.2%～103.6%,相对标准偏差为4.4%～8.0%;DAP的回收率为79.4%～106.8%,相对标准偏差为2.0%～4.0%。HAP在5.4～216.4滋g/L范围内具有良好线性关系（r≥0.999）;DAP在4.1～164.2滋g/L范围内具有良好线性关系。[结论]该HAP和DAP的高液相色谱分析方法,可以满足国际上对多菌灵、苯菌灵、甲基硫菌灵原药中的有害杂质的检测限定要求。

[Aims] The high performance liquid chromatography coupled with UV detector was employed for the determination of 2-hydroxy-3-aminophenazine （HAP） and 2,3-diaminophenazine （DAP） in carbendazim, benomyl and thiophanate-methyl technical. [Methods] The technical samples were analyzed by using Hypersil ODS column and UV detector at 453 nm, with gradient elution of methanol and KH2PO4 aqueous buffer solution （pH 8） as the mobile phase. [Results] The recoveries of HAP were between 89.2 and 103.6%, with RSD varied from 4.4 to 8.0%. The recoveries of DAP were between 79.4 and I06.8%, with RSD varied from 2.0 to 4.0%. The linear correlation coefficient for HAP and DAP were above 0.999 with the concentration 5.4-216.4 μg/L and 4.1-164.2μg/L, respectively. [Conclusions] The high performance liquid chromatographic analysis method can satisfy the requirements of international limit content for HAP and DAP.