顶空毛细管气相色谱法测定奥硝唑原料的溶剂残留

Determination of the residual solvents in ornidazole by headspace capillary GC

目的建立奥硝唑原料药中5种有机溶剂残留量的顶空毛细管气相色谱测定法。方法使用Agilent DB-624毛细管气相色谱柱（30m×0.32mm×0.18μm）,FID检测器,进样口温度150℃,检测器温度250℃。程序升温45℃,保持15min,然后以40℃·min-1的速率升至220℃。顶空进样,平衡温度85℃,平衡时间30min。结果在上述条件下,甲醇,乙醇,乙酸乙酯,二氯乙烷和环氧氯丙烷的分离度均在2.0以上,线性关系良好（r在0.997 8~0.999 9之间）,平均回收率（n=6）在100.9%~103.4%之间,RSD在1.4%~3.3%之间。结论该法简单、准确,可用于奥硝唑原料中残留溶剂的测定。

Objective To optimize the extraction and preparation process of Gedanlan Capsules .Method An orthogonal experimental design was used to optimize the parameters of the extraction process on the basis of the dry extract yield and flavonoid contents , and the single factor experiment was used to optimize the parameters of the preparation process .Results Ginseng was crushed and the resulting powder was used . Pueraria lobata radix ,Salvia miltiorrhiza ,Lolium mori and Gynostemma pentaphyllum were extracted for two times with 70% ethanol ,the ratio of solvent to material was 12 ,the extraction time was 1 .5 h ,and the resulting extraction liquid was condensed into a dry paste for use .The ginseng powder and the dry paste powder were mixed with 85% eth‐anol for soft material ,and the granule was prepared by 16 mesh sieve and filled into the No .0 capsule for Gedanlan Capsules . Conclusion The preparation of Gedanlan Capsules is feasible .