【摘要】 采用气相色谱法在5%siliconOV-7/ChromosorbW-AWDMCS(0.231～0.387mm)色谱柱上分离和测定药物中间体3-氨基-2-噻吩甲酸甲酯。在选定的色谱条件下,3-氨基-2-噻吩甲酸甲酯与内标物邻苯二甲酸二乙酯及杂质之间具有较好的分离效果;并以邻苯二甲酸二乙酯为内标物时,3-氨基-2-噻吩甲酸甲酯的相对重量校正因子相当稳定,即fw,A=1.83。该方法操作简便、快速,精密度和准确度较好。对同一试样的五次平行测定的标准偏差为0.66%,相对标准偏差为1.59%;该方法的标准加入回收率98.61%～102.8%。更多还原

【Abstract】 The separation and determination of medicine intermediate methyl 3-amino-2-thiophenecarboxylate were studied by gas chromatography on the 5% silicon OV-7/Chromosorb W-AW DMCS. Under the selected chromatographic conditions, the resolution between methyl 3-amino-2-thiophenecarboxylate and the internal standard diethyl phthalate and impurities was good. Diethyl phthalate is used as an internal standard for the determination of 3-amino-2-thiophenecarboxylate with a correction factor of 1.83. It is a simple, fast, and accurate method for the determination of methyl 3-amino-2-thiophenecarboxylate. For the five parallel analyses of a same sample, the standard deviation of this method was 0.66% with a coefficient variation of 1.59%. The recovery of methyl 3-amino-2-thiophenecarboxylate was 98.61%～102.8%更多还原