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

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。

Objective:To develop purity reference material of tetracycline and identify its impurities.Methods:Ultra performance liquid chromatography (UPLC)with high resolution time of flight mass spectrometry (HRTOF/MS)was employed for qualitative determination of tetracycline and its impurities.The checking of uniformity,the stability test and the value certification were systematically studied by HPLC.And the uncertainty was evaluated.Results:The main component and 4 kinds of impurities were confirmed by UPLC-HRTOF/MS.The impurities were epitetracycline,chlortetracycline,epianhydrotetracycline and anhydrotetracycline.The certified value of the reference material of tetracycline purity was 95.6% with the expanded uncertainty of 1.1% (k=2).The long-term stability results showed that tetracycline was stable within 12 months stored at-20℃ in darkness.Conclusion:The uniformity and stability of the reference material can meet the technical requirement of the standard reference material.And it can be used to provide technical support and guarantee traceability for food inspection,health inspection and other aspects of scientific researches.