高效液相色谱法测定尿素的有关物质  

Determination of related substances in the urea by HPLC

作　　者：李颖 谢莹莹 郑金凤 张悦 赵勇 刘杨 蒋赟 LI Ying;XIE Ying-ying;ZHENG Jin-feng;ZHANG Yue;ZHAO Yong;LIU Yang;JIANG Yun(Hunan Institute of Drug Control,Changsha 410001;Hunan Drug Inspection Center,Changsha 410001;NMPA Key Laboratory for Pharmaceutical Excipients Engineering Technology Research,Changsha 410001)

机构地区：[1]湖南省药品检验检测研究院,长沙410001 [2]湖南省药品审查核验中心,长沙410001 [3]国家药品监督管理局药用辅料工程技术研究重点实验室,长沙410001

出　　处：《中南药学》2022年第8期1902-1906,共5页Central South Pharmacy

基　　金：湖南省自然科学基金项目(No.2021JJ80034)。

摘　　要：目的建立高效液相色谱法测定尿素的有关物质。方法采用Waters XBridge Amide(4.6 mm×250 mm,3.5μm)色谱柱,以乙腈-水(94∶6)为流动相,流速1.0 mL·min^(-1),柱温30℃,检测波长195 nm,进样量10μL。结果在该色谱条件下,缩二脲、缩三脲、三聚氰酸和尿素之间能完全分离;尿素中缩二脲、缩三脲、三聚氰酸分别在0.4966~19.8665μg·mL^(-1)、0.5375~21.5028μg·mL^(-1)和0.5842~23.3710μg·mL^(-1)与峰面积线性关系良好,相关系数分别为1.000、0.9999和0.9998,平均回收率分别为100.1%、100.3%、86.59%,RSD分别为1.4%、0.44%、3.3%(n=6),供试品溶液在12 h内稳定。结论本方法准确度高、重现性好,可用于尿素中有关物质的测定,为建立尿素的质量标准提供参考。Objective To determine the related substances in the urea by HPLC.Methods Waters XBridge Amide(4.6 mm×250 mm,3.5μm)chromatographic column was used,with acetonitrilewater(94∶6)as the mobile phase.The flow rate was 1.0 mL·min^(-1),the column temperature was 30℃,the detection wavelength was 195 nm,and the injection volume was 10μL.Results Under this chromatographic condition,biuret,triuret,cyanuric acid and urea were completely separated.Biuret,triuret,and cyanuric acid in the urea showed good linearity at 0.4966~19.8665μg·mL^(-1),0.5375~21.5028μg·mL^(-1) and 0.5842~23.3710μg·mL^(-1) respectively,with the correlation coefficients of 1.000,0.9999 and 0.9998 respectively.The average recovery was 100.1%,100.3%,and 86.59%,and the RSD was 1.4%,0.44%,and 3.3%(n=6),respectively.The test solution was stable within 12 h.Conclusion This method has high accuracy and good reproducibility,which can be used for the determination of related substances in the urea,and provide a reference for the quality standard of urea.

关 键 词：尿素 高效液相色谱法 缩二脲 缩三脲 三聚氰酸 

分 类 号：R927[医药卫生—药学]