摘要
目的 建立起琥宁有机溶剂残留量的测定方法。方法 采用气相色谱法,色谱柱为2m×3mm不锈钢色谱柱,柱填料为GDX-102(60-80目);FID检测器;按外标法同时测定炎琥宁合成过程中涉及的乙醇、丙酮和吡啶的残留量。结果 在该色谱条件下,测得各溶剂线性均良好(r=0.9996~0.9999);平均回收率分别为97.86%,98.16%和98.04%;RSD分别为0.5%,0.8%和0.8%;乙醇、丙酮和吡啶的最低检测限分别为0.005%,0.005%和0.002%;3批样品中上述有机溶剂残留量均符合要求。结论 该方法简单、快捷、灵敏,可有效用于炎琥宁有机溶剂残留量的控制。
Objective To establish the analysis methods for the residual ethanol, acetone and pyridine in potassium sodium dehydroandroan drographolide succinate samples with capillary gas chromatography. Methods Commercially available and selfprepared samples were analyzed on a gas chromatograph using flame ionization detector with a capillary column (200 mm×3 mm; GDX-102). Results Good linear correlations were obtained during the detection ( r = 0. 999 6-0. 999 9). The average recoveries were 97. 86% (RSD was 0.5%, n = 5 ) ,98. 16% (RSD was 0.8%, n = 5 ) and 98. 04% (RSD was 0.8%, n = 5 ) for ethanol, acetone and pyridine, respectively. The limits of quantification for ethanol, acetone an pyridine were 0. 005% , 0.005% and 0. 002%, respectively. The contents of the residual solvents in three batches of products were acceptable. Conclusion The method is reliable and can be applicable in the detection of residual ethanol, acetone and pyridine in potassium sodium dehydroandroan drographolide succinate samples.
出处
《时珍国医国药》
CAS
CSCD
北大核心
2006年第4期572-573,共2页
Lishizhen Medicine and Materia Medica Research
关键词
炎琥宁
有机溶剂残留量
气相色谱法
Potassium sodium
Dehydroandroan drographolide succinate
Gas chromatography