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頂空氣相色譜法測定鹽酸頭孢替安酯原料藥中殘留溶劑含量

發(fā)布時間:2018-02-21 10:01

  本文關(guān)鍵詞: 頭孢替安酯 鹽酸 色譜法 氣相 頂空采樣 殘留溶劑 出處:《醫(yī)藥導(dǎo)報》2016年02期  論文類型:期刊論文


【摘要】:目的建立頂空氣相色譜法同時測定鹽酸頭孢替安酯原料藥中丙酮、乙酸乙酯、異丙醇、二氯甲烷、乙腈5種殘留溶劑。方法采用Agilent DB-624(6%氰丙基苯基-94%二甲基聚硅氧烷固定相)石英毛細(xì)管柱(30 m×0.53 mm,3.0μm),火焰離子化檢測儀(FID)檢測器,N,N-二甲基甲酰胺(DMF)為溶劑。結(jié)果 5種殘留溶劑在各自的濃度范圍內(nèi)呈現(xiàn)良好的線性關(guān)系(r=0.999 6~0.999 9,n=5),最低檢出限范圍為0.071~0.847μg;5種殘留溶劑檢測的穩(wěn)定性RSD為0.40%~2.12%(n=3),平均加樣回收率為99.03%~104.79%,RSD為0.54%~3.41%(n=3)。結(jié)論該方法簡單、靈敏、可靠,適用于鹽酸頭孢替安酯原料藥中殘留溶劑的分析檢測。
[Abstract]:Objective to establish a headspace gas chromatography method for the simultaneous determination of acetone, ethyl acetate, isopropanol and dichloromethane in ceftianil hydrochloride. Five residual solvents of acetonitrile were used. Methods Agilent DB-624A6% cyanopropyl phenyl 94% dimethyl polysiloxane stationary phase) quartz capillary column (30 m 脳 0.53 mm ~ (3) 渭 m) and flame ionization detector (FID) were used as solvent. There was a good linear relationship between the residual solvents in their respective concentration ranges. The lowest detection limit was 0.071 ~ 0.847 渭 g ~ (-1) 渭 g ~ (-1). The RSD was 0.40 ~ 2.12% and the average recovery was 99.03 ~ 104.79 ~ 0.54 ~ 3.41 渭 g ~ (-1) 渭 g ~ (-1). Conclusion the method is simple, and the relative standard deviation is 0.54 ~ (3.41) 渭 g ~ (-1) for the determination of residual solvents. It is sensitive, reliable and suitable for the determination of residual solvent in ceftiamil hydrochloride.
【作者單位】: 抗生素研究與再評價四川省重點(diǎn)實(shí)驗(yàn)室成都大學(xué)四川抗菌素工業(yè)研究所;成都軍區(qū)總醫(yī)院藥劑科;
【基金】:成都大學(xué)自然科學(xué)青年基金(2080515057)
【分類號】:R927.2;O657.71
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本文編號:1521671

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