| 李茜,刘英,姚永青.顶空气相色谱法测定醋酸奥曲肽原料中的残留溶剂[J].中国药品标准,2016,17(6):420-423 |
| 顶空气相色谱法测定醋酸奥曲肽原料中的残留溶剂 |
| Determination of Residual Solvents in Octreotide Acetate Raw Material by Headspace Gas Chromatography |
| 投稿时间：2016-05-06 修订日期：2016-11-01 |
| DOI： |
| 中文关键词: 醋酸奥曲肽 残留溶剂 顶空气相色谱法 |
| 英文关键词: Octreotide Acetate residual solvent headspace gas chromatography |
| 基金项目: |
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| 摘要点击次数: 588 |
| 全文下载次数: 280 |
| 中文摘要: |
| 目的：采用顶空气相色谱法测定醋酸奥曲肽原料中的残留溶剂。方法：采用6%腈丙基苯基-94%二甲基聚硅氧烷(DB-624)毛细管色谱柱(30 m×0.32 mm×0.25 μm)，柱温为程序升温：初始温度为40 ℃，保持4 min，然后以20 ℃?min-1的升温速率升至200 ℃，保持15 min，进样口温度200 ℃，氢火焰离子化检测器，检测器温度280 ℃，分流比2:1，载气流速为1.0 mL?min-1。结果：4种残留溶剂均能完全分离，甲醇、乙腈、二氯甲烷、N,N-二甲基甲酰胺线性范围分别为19.89～318.18mg?mL-1 (r=0.999 7)、4.19～67.07mg?mL-1 (r=0.999 7)、11.69～58.44mg?mL-1 (r=0.999 7)和20.38～122.28mg?mL-1 (r=0.999 7)；检测限分别为1.30、0.03、0.02μg和3.76μg。结论：该方法重复性好，灵敏度高，可用于醋酸奥曲肽原料中的残留溶剂控制。 |
| 英文摘要: |
| Objective: To establish a headspace GC method for the content deternination of residual solvents in Octreotide Acetate raw material. Methods: A DB-624 capillary column (30 m×0.32 mm×0.25 μm) was used and column temperature was programmed heating up. The initial temperature was kept at 40℃ for 4 min, then the temperature was raised to 200℃ at the rate of 20 ℃?min-1 and kept for 15min. The inlet temperature was 200 ℃, FID detector temperature was 280 ℃, the split ratio was 2:1 and the carrier gas flow rate was 1.0 mL?min-1. Results: 4 residual solvents were separated completely, the linear ranges of methanol, acetonitrile, dichloromethane and N,N- dimethylformamide were 19.89–318.18mg?mL-1 (r=0.999 7),4.19–67.07mg?mL-1 (r=0.999 7),11.69–58.44mg?mL-1 (r=0.999 7) and20.38–122.28mg?mL-1 (r=0.999 7),respectively. The detection limits of them were 1.30, 0.03, 0.02μg and 3.76μg. Conclusion: The method is repeatable and sensitive for the quality control of residual solvents in Octreotide Acetate raw material. |
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