毛细管气相色谱法测定药品硝酸硫胺中有机溶剂残留量的研究

Analysis and determination of residual organicsolvents in pharmaceuticals(thiamine nitrate) by capillary gas chromatography

建立了测定药品硝酸硫胺中含有的中国药典规定的前3类有机溶剂含量的方法,以确定它们在药物中的残留量和比例.实验方法采用毛细管气相色谱法,首先采用GC-MS对样品进行扫描定性,再应用离子火焰检测器（FID）对残留的有机溶剂进行定量,应用顶空和直接进样两种方式采集数据,以DB-624色谱柱（30 m×250μm×1.4μm）对样品进行分离,采取程序升温,载气为氦气,外标法计算含量.结果显示：在各色谱条件下,测得各溶剂的线性良好（R^2〉0.90）,平均回收率为95.32%-99.25%,RSD为3.72%-7.35%,最低检出限为1.78×10^-6-1.45×10^-5;所测试药品中除甲醇、丁酮、乙酸3种有机溶剂有检出外,其他都未检出.

A method for determining contents of first three kinds of residual organic solvents which stipulated in Chinese pharmacopoeia in pharmaceuticals（thiamine nitrate） was established by capillary gas chromatography.The experimental conditions were DB-624 silica capillary column,MSD and FID detector,HS and ALS mode,carrier helium gas and external standard calibration method.The results indicated that the residual organic solvents were separated completely and the linearity was well（R^2〉0.99）.Average recovery was 95.32%—99.25%,RSD was 3.72%—7.35%.The lowest detection limit was 1.78×10^-6—1.45×10^-5.Only methanol,butanone and acetic acid solvents were detected in the thiamine nitrate,but other solvents were no done.