| 引用本文: | 王建,王红波,王知坚.GC测定盐酸克林霉素棕榈酸酯中的9种残留溶剂[J].中国现代应用药学,2012,29(9):829-833. |
| WANG Jian,WANG Hongbo,WANG Zhijian.Determination of Nine Residual Organic Solvent in Clindamycin Palmitate Hydrochloride by GC[J].Chin J Mod Appl Pharm(中国现代应用药学),2012,29(9):829-833. |
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| 摘要: |
| 目的 建立毛细管气相色谱法测定盐酸克林霉素棕榈酸酯中的残留溶剂。方法 乙醇、丙酮、乙腈、二氯甲烷、乙酸乙酯和三氯甲烷测定采用顶空进样法，色谱柱为DB-624(6%氰丙基苯基-94%二甲基聚硅氧烷固定液)石英毛细管柱，柱温为60 ℃，维持10 min，以20 ℃·min-1升至180 ℃，维持2 min，二甲基甲酰胺-水(1∶4)为溶剂；甲苯、吡啶和二甲基甲酰胺测定采用直接进样法，色谱柱为DB-624(6%氰丙基苯基-94%二甲基聚硅氧烷固定液)石英毛细管柱，柱温为90 ℃，二氯甲烷为溶剂。结果 被测物均能得到很好的分离，峰面积与浓度呈良好的线性关系，精密度和回收率良好。结论 该法可用于盐酸克林霉素棕榈酸酯原料药中残留溶剂的检测。 |
| 关键词: 盐酸克林霉素棕榈酸酯 气相毛细管色谱法 残留溶剂 顶空进样 直接进样 |
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| 基金项目:国家药典委员会国家药品标准提高研究项目(国药典化发[2010]84号) |
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| Determination of Nine Residual Organic Solvent in Clindamycin Palmitate Hydrochloride by GC |
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WANG Jian1, WANG Hongbo2, WANG Zhijian1
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1.Zhejiang Institute for Drug Control, Hangzhou 310004, China;2.Zhejiang University of Technology, Hangzhou 310014, China
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| Abstract: |
| OBJECTIVE To establish a method of capillary gas chromatography for the determination of residual solvents in clindamycin palmitate hydrochloride. METHODS Ethanol, acetone, acetonitrile, dichloromethane, acetic ether and trichlormethane were separated on DB-624 capillary column through head-space sampling mode. The column temperature was maintained at 60 ℃ for 10 min, then was raised to 180 ℃ at the rate of 20 ℃·min-1 and maintained at 180 ℃ for 2 min. The sample was dissolved in dimethylformamide-water (1∶4). Pyridine, toluene and dimethylformamide were separated on DB-624 capillary column through direct sampling mode. The column temperature was 90 ℃. The sample was dissolved in dichloromethane. RESULTS The measured solvents were separated completely. The calibration curve of each solvent showed a good linear relationship with precision and accuracy. CONCLUSION The established method is simple, reliable, which can be used for determination of residual solvents in clindamycin palmitate hydrochloride. |
| Key words: clindamycin palmitate hydrochloride GC residual organic solvents head-space sampling direct sampling |
