【摘要】 [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。更多还原

【Abstract】 [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 106.8%,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 4.1-164.2 μg/L,respectively. [Conclusions] The high performance liquid chromatographic analysis method can satisfy the requirements of international limit content for HAP and DAP.更多还原