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期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nicpbp.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237
 

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UHPLC-MS/MS法同时测定六合氨基酸注射液中6个有效成分的含量

Simultaneous determination of six active components in compound amino acid injection by UHPLC-MS/MS

作者: 王清华 
作者(英文):
分类号:R917
出版年·卷·期(页码):2019,39 (2):257-262
DOI: 10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------

目的:建立UHPLC-MS/MS法同时检测六合氨基酸注射液中6个有效成分(L-精氨酸、L-谷氨酸、L-门冬氨酸、L-亮氨酸、L-异亮氨酸和L-缬氨酸)的含量。方法:采用Agilent ZORBAX SB-C18(3.0mm×150 mm,5 μm)色谱柱分离,以含0.2%甲酸和0.02%七氟丁酸的甲醇溶液-含0.2%甲酸和0.02%七氟丁酸的水溶液为流动相,梯度洗脱,流速0.4 mL·min-1,柱温50℃;以电喷雾离子源(ESI),正离子扫描方式,多反应监测扫描模式进行定量分析。结果:所测6个氨基酸浓度在一定范围内呈良好的线性关系,r>0.999 3;实验精密度、稳定性、重复性良好;平均加样回收率为95.8%~103.2%,RSD<4.2%。10批样品中L-精氨酸、L-谷氨酸、L-门冬氨酸、L-亮氨酸、L-异亮氨酸和L-缬氨酸的含量检测结果分别为21.64~22.24、18.12~18.64、3.84~4.24、16.40~16.88、10.76~11.48和11.96~12.48 mg·mL-1结论:经方法学验证,所建立的分析方法简便、快速、准确,灵敏度高,可作为六合氨基酸注射液的质量控制和评价方法。  

-----英文摘要:---------------------------------------------------------------------------------------

Objective: To establish a method for simultaneous determination of six effective components (L-arginine, L-glutamic acid, L-aspartic acid, L-leucine, L-isoleucine and L-valine) in the compound amino acid injection by UHPLC-MS/MS. Methods: Separation was performed on an Agilent Zorbax SB-C18 column (3.0 mm×150 mm, 5 μm) using a linear gradient solvent system of methanol(0.2% formic acid and 0.02% heptafluorobutyric acid) and water(0.2% formic acid and 0.02% heptafluorobutyric acid) as mobile phase, at a flow rate of 0.4 mL·min-1 and the column temperature was set at 50℃. Detection was executed by MS/MS in the multiple reaction monitoring(MRM) mode using a positive electrospray ionization interface. Results: This method exhibited excellent linearity for all of the analytes with regression coefficients r>0.999 3. The precision,stability, and repeatability of the method were good for all the six amino acids. The average recoveries varied between 95.8% and 103.2%,with the RSD were less than 4.2%. The components of L-arginine,L-glutamic acid,L-aspartic acid, L-leucine, L-isoleucine and L-valine in 10 samples were 21.64~22.24,18.12~18.64, 3.84~4.24, 16.40~16.88, 10.76~11.48 and 11.96~12.48 mg·mL-1, respectively. Conclusion: The method was proved to be convenient, accurate, sensitive and good in reproducibility, which could be applied to the quality control and assessment of compound amino acid injection. 

-----参考文献:---------------------------------------------------------------------------------------

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