六味生物制剂有效部位残留正丁醇去除工艺优选及正丁醇残留量检测

Optimal Technique for Eliminating n-Butanol and Determination of n-Butanol Residue in Active Composition of LW-PSB

目的建立六味生物制剂有效部位正丁醇残留量的检测方法,确定六味生物制剂有效部位残留正丁醇的最佳去除工艺。方法运用气相色谱法测定正丁醇残留量,以正丁醇残留量为考察指标,结合正交试验设计,优选最佳的残留正丁醇去除工艺。结果正丁醇残留量检测方法平均回收率为99.62%,RSD为2.05%。六味生物制剂有效部位残留正丁醇的最佳去除工艺为每次加入0.5倍量水,80℃旋转蒸发3次,测得正丁醇残留量符合《中国药典》规定限量标准。结论本试验所建立的正丁醇残留量检测方法准确可靠,优选的正丁醇去除工艺简便可行,为后续产品研发奠定基础。

Objective To establish a method for detecting residual n-butanol and to optimize the process for eliminating n-butanol in active composition of LW-PSB. Methods We detected the residual n-butanol in active compositions of LW-PSB by gas chromatography（GC）, and optimized the process condition for the elimination of nbutanol with residual n-butanol as the indexes and by using the orthogonal experimental design. Results The recovery of residual n-butanol was 99.62 % with RSD being 2.05 %. The optimal process for eliminating n-butanol was adding 0.5-fold water every time and reduced-pressure distillation at 80 ℃ for three times, and the obtained residual nbutanol level was in accordance with the pharmacopeial limit. Conclusion The method for detecting residual nbutanol in active composition of LW-PSB is accurate and reliable. The optimal technique is convenient and practical, and will lay a good foundation for the product development.