1顶空毛细管气相色谱法测定盐酸丁卡因原料药中的残留溶剂
Head-space sampling CGC determination of residual solvents in raw material drug of tetracaine hydrochloride
分类号:
出版年·卷·期(页码):2011,31 (6):0-0
DOI:
10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------
目的: 建立了顶空毛细管气相色谱法同时测定盐酸丁卡因原料药中乙醇、乙酸乙酯、正丁醇、溴丁烷、N,N-二甲基乙酰胺等5种残留溶剂的分析方法。 方法: 采用Agilent DB-624毛细管色谱柱(30 m×0.53 mm×3.0 μm),FID检测器,二甲基亚砜(DMSO)为溶剂。 结果: 5种残留溶剂在各自的浓度范围内呈良好的线性关系(r=0.99882~0.99994,n=8),最低检出限范围为1.2~112 μg·g-1;5种残留溶剂检测的日间稳定性(以RSD)计)为0.5%~2.2% (n=3),3种加标浓度的平均添加回收率为94.9%~105.6% (RSD为0.6%~3.4%,n=3)。 结论: 本方法简单、灵敏、可靠,适用于盐酸丁卡因原料药中残留溶剂的分析检测。
-----英文摘要:---------------------------------------------------------------------------------------
Objective: A capillary GC method with head-space sampling was established for determination of residual solvents—Ethanol,Ethyl acetate,n-Butanol,1-Bromobutane and N,N-dimethylacetamide in raw material drug of tetracaine hydrochloride. Method: Agilent DB-624 capillary column(30 m×0.53 mm×3.0 μm) was used,with FID as detector and DMSO as the solvent. Result: Linear responses were obtained for the 5 residual solvents in their respective concentration ranges (r=0.99882-0.99994,n=8),and the limits of detection were 1.2-112 μg·g-1.The inter-day stabilities,measured as relative standard deviations(RSDs),were 0.5%-2.2% (n=3).The average recoveries of three concentration levels were 94.9%-105.6% with the RSD of 0.6%-3.4%(n=3). Conclusion: The developed method is simple,sensitive,and accurate for the residual solvent analysis in raw material drug of tetracaine hydrochloride.
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