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目的:建立一种适用于新型alpha芋螺镇痛多肽Eb1.6含量及有关物质的分析方法,以及其水分和乙酸的含量测定方法。方法:采用高效液相色谱法测定Eb1.6原料药中Eb1.6的含量。使用Zorbax XDB-C18色谱柱(150 mm×4.6 mm,5μm),流动相A为含0.1%三氟乙酸(TFA)的水,流动相B为含0.1%TFA的乙腈,梯度洗脱,流速1 m L·min-1,检测波长214 nm,柱温25℃;采用卡尔菲休库仑滴定法及高效液相色谱法测定样品中水分及乙酸含量。结果:3批Eb1.6原料药中Eb1.6含量范围在(98.85±0.63)%~(99.04±0.33)%之间(按无水物计算),总有关物质含量在0.45%~0.84%之间,样品中水分含量在(1.23±0.32)%~(2.23±0.23)%之间,乙酸含量在(11.16±0.08)%~(12.66±0.03)%之间。结论:该方法快速简便,结果准确可靠,可用于Eb1.6的质量分析。
OBJECTIVE: To establish a method for the determination of Eb1.6 and its related substances in a new type of alpha-taro analgesic peptide, and to determine its content of water and acetic acid. Methods: The content of Eb1.6 in Eb1.6 drug substance was determined by high performance liquid chromatography. The mobile phase A was water containing 0.1% trifluoroacetic acid (TFA) and the mobile phase B was acetonitrile containing 0.1% TFA using a Zorbax XDB-C18 column (150 mm × 4.6 mm, 5 μm) m L · min-1, the detection wavelength was 214 nm and the column temperature was 25 ℃. The contents of water and acetic acid in the samples were determined by Coulometric coulometric titration and high performance liquid chromatography. Results: The content of Eb1.6 in the three batches of Eb1.6 APIs ranged from (98.85 ± 0.63)% to (99.04 ± 0.33)% (calculated on anhydrous basis) with the total content of related substances ranging from 0.45% to 0.84% The water content in samples was between (1.23 ± 0.32)% and (2.23 ± 0.23)% and the acetic acid content was between (11.16 ± 0.08)% and (12.66 ± 0.03)%. Conclusion: The method is rapid and simple, accurate and reliable, and can be used for quality analysis of Eb1.6.