摘要
建立了在5％ OV-7/Chromosorb W-AW DMCS气相色谱柱上分离和测定药物中间体2-乙酰噻吩的方法。在选定的色谱条件下,2-乙酰噻吩与内标物草酸二乙酯及杂质之间具有较好的分离效果。以草酸二乙酯为内标物时,2-乙酰噻吩的质量校正因子(g_(w.A)=0.63)相当稳定。当2-乙酰噻吩与草酸二乙酯的质量比(X)为0.02～1.82时,2-乙酰噻吩与草酸二乙酯的峰面积比(Y)与其质量比(X)之间具有较好的线性关系,其线性回归方程为Y=1.491X+0.0577,相关系数r=0.9984。方法的相对标准偏差为1.81％,回收率为96.96％～98.36％。
The method of the determination of drug intermediate 2-acetylthiophene was set up by gas chromatography on 1 500 mm ×3mm i.d. packed with Chromosorb W - AW DMCS (0. 175 -0. 246 mm) coated with 5 % OV-7. Under the selected chrom-atographic conditions, the separation efficiency between 2-acetylthiophene and internal standard diethyl oxalate and impurities was better. Diethyl oxalate is used as internal standard for determination of 2-acetylthiophene with correction factor of 0.63. When the quality ratio between 2-acetylthiophene and diethyl oxalate was 0.02 - 1. 82, the relationship of quality and peak area ratio between 2-acetylthiophene and diethyl oxalate possessed better linearity, namely, linearity equation follows as Y= 1. 491X + 0. 0577 (r =0. 9984). The relative standard deviation of the method was 1.81%. The recovery was 96. 96% -98. 36%.
出处
《化学分析计量》
CAS
2002年第1期10-12,共3页
Chemical Analysis And Meterage
关键词
2-乙酰噻吩
药物中间体
气相色谱
分离
测定
分析
2-acetylthiophene, drug intermediate, gas chromatography, separation, determination
