超高效液相色谱-高分辨飞行时间质谱鉴定四环素杂质及纯度标准物质的研制

发布时间：2018-02-01 00:15

  本文关键词： 四环素 纯度标准物质 杂质鉴定 差向四环素 金霉素 脱水四环素 差向脱水四环素 高效液相色谱-质谱 稳定性 不确定度　出处：《药物分析杂志》2015年11期 　论文类型：期刊论文

【摘要】：目的:研制兽药四环素的纯度标准物质并对其杂质进行鉴定;方法:采用超高效液相色谱-高分辨飞行时间质谱(UPLC-HRTOF/MS)对四环素及其杂质进行定性分析,采用高效液相色谱法对四环素标准物质进行定值以及均匀性和稳定性检验,并对标准值的不确定度进行评估。结果:UPLC-HRTOF/MS鉴定出四环素中的4种杂质,分别为差向四环素、金霉素、差向脱水四环素和脱水四环素。四环素纯度标准物质定值结果为95.6%,扩展不确定度为1.1%(k=2)。在-20℃下避光保存可以保证在12个月内量值稳定。结论:四环素标准物质符合国家标准物质的技术要求,可为食品检验、卫生检验检疫、科学研究等方面的测量和研究工作提供技术支撑和量值溯源保障。
[Abstract]:Objective: to prepare the purity standard substance of veterinary drug tetracycline and to identify its impurity. Methods: the tetracycline and its impurity were qualitatively analyzed by UPLC-HRTOF / MS by ultra-high performance liquid chromatography-high resolution time-of-flight mass spectrometry. The determination, uniformity and stability of tetracycline reference materials were determined by high performance liquid chromatography (HPLC). The uncertainty of the standard value was evaluated. Results the four impurities in tetracycline were identified as differential tetracycline and chlortetracycline. Differential dehydration tetracycline and dehydrated tetracycline. The purity of tetracycline is determined to be 95.6%. The extended uncertainty is 1.1 / kg ~ 2 ~ (2). The quantity of tetracycline can be kept stable within 12 months by keeping away from light at -20 鈩，

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