| 引用本文: | 刘峰,赵荣丽,袁军.顶空气相色谱法测定聚普瑞锌中的残留溶剂[J].中国现代应用药学,2016,33(2):193-196. |
| LIU Feng,ZHAO Rongli,YUAN Jun.Determination of Residual Organic Solvents in Sevelamer Hydrochloride Drug Substance by Headspace Gas Chromatography[J].Chin J Mod Appl Pharm(中国现代应用药学),2016,33(2):193-196. |
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| 摘要: |
| 目的 建立以顶空气相色谱法测定聚普瑞锌原料药中甲醇、乙醇、三氯甲烷和甲苯4种有机溶剂残留量的方法。方法 以1 mol·L-1硫酸溶液为溶剂，采用Agilent DB-FFAP(30 m×0.32 mm，0.5 μm)毛细管柱，载气为氮气，柱流速为2 mL·min-1；柱温为程序升温，氢火焰离子化检测器(FID)，检测器温度为250 ℃；进样口温度为200 ℃；顶空瓶平衡温度为80 ℃。结果 甲醇、乙醇、三氯甲烷和甲苯均能较好的分离，呈现良好的线性关系，平均回收率分别为102.9%，105.4%，93.8%，95.7%，RSD分别为2.9%，2.1%，3.3%，3.5%(n=9)。结论 本方法简便快速，准确性好，灵敏度高，可用于聚普瑞锌原料药中残留溶剂的测定，同时也为难溶性原料药中的残留溶剂测定提供一个思路。 |
| 关键词: 顶空气相色谱法 聚普瑞锌 残留溶剂 |
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| Determination of Residual Organic Solvents in Sevelamer Hydrochloride Drug Substance by Headspace Gas Chromatography |
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LIU Feng1,2, ZHAO Rongli3, YUAN Jun2
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1.State Key Laboratory of Biotherapy, Sichuan University, Chengdu 610041, China;2.Sichuan Institute for Food and Drug Control, Chengdu 610097, China;3.Chengdu Institute of Biological Products, Chengdu 610023, China
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| Abstract: |
| OBJECTIVE To establish an HS-GC method for the determination of residual organic solvents including menthanol, alcohol, trichloromethane and toluene in polaprezinc. METHODS The samples were dissolved in 1 mol·L-1 sulfuric acid solution, and this method utilized an Agilent DB-FFAP GC column, nitrogen as carrier gas. FID was used as detector with the temperature of 250 ℃, and the inlet temperature was 200 ℃. This method used temperature program. RESULTS The four residual organic solvents menthanol, alcohol, trichloromethane and toluene were completely separated, the linear relationship was good, and the average recoveries were 102.9%, 105.4%, 93.8% and 95.7%, and the RSD were 2.9%, 2.1%, 3.3%, 3.5%(n=9), respectively. CONCLUSION This method is simple, rapid, accurate and highly sensitive, which can be used for the determination of the residual organic solvents in polaprezinc. Also provide a way of determination of residual organic solvents in slightly soluble crude drug. |
| Key words: HS-GC polaprezinc residual organic solvents |
