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气相色谱法测定富马酸替诺福韦二吡呋酯中三乙胺残留量
Determination of Residual Triethylamine in Tenofovir Disoproxil Fumarate by GC
投稿时间:2014-11-23  修订日期:2015-01-04
DOI:
中文关键词:  气相色谱法  三乙胺  富马酸替诺福韦二吡呋酯
英文关键词:GC  Triethylamine  Tenofovir disoproxil fumarate
基金项目:国家“重大新药创制”科技重大专项(编号:2009ZX09301-013)
作者单位
张治云 山东省药学科学院 山东省生物药物重点实验室 济南 250101山东福瑞达医药集团公司 山东省黏膜与皮肤给药技术重点实验室 
毋立华 山东省药学科学院 山东省生物药物重点实验室 
邢玉仁 山东省药学科学院 山东省生物药物重点实验室 
刘荣磊 山东省药学科学院 山东省生物药物重点实验室 
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中文摘要:
      摘 要 目的: 建立富马酸替诺福韦二吡呋酯中三乙胺残留的检测方法。方法: 采用气相色谱法,色谱柱为安捷伦DB-624毛细管柱(30 m×0.53 mm,3 μm),氢火焰离子化检测器(FID),载气为氮气,流速2.0 ml·min-1,柱温采用程序升温,初始温度为50℃,以10℃·min-1升温至220℃,保持4 min,采用外标法定量。结果:三乙胺浓度在53.02~742.34 μg·mL-1的范围内,峰面积和浓度呈现良好的线性关系,相关系数为0.999 8;回收率为96.52%~102.27%,RSD为2.42%(n=9)。结论: 本法专属性强、重复性好、灵敏度高,可用于富马酸替诺福韦二吡呋酯中三乙胺残留测定。
英文摘要:
      ABSTRACT Objective: To establish a method for the determination of residual triethylamine in tenofovir disoproxil fumarate. Methods: The residual treithylamine was determined by GC with an Agilent DB-624 capillary column (30 m×0.53 mm, 3 μm) and an FID detector. The carrier gas was nitrogen and the flow rate was 2.0 ml·min-1. The oven temperature was programming increased. The initial column temperature was 50℃, and then raised to 220℃ at a rate of 10℃·min-1,and maintained 4 min. Triethylamine was quantified by an external standard.Results: The calibration showed a good linearity within the range of 53.02-742.34 μg·mL-1 for triethylamine. The correlation coefficient was 0.999 8. The recoveries were within the range of 96.52%-102.27%. The relative standard deviation (RSD) was2.42% (n=9). Conclusion:The method has good specificity,repeatability and sensitivity, which can be used in determining the content of residual trietbylamine in tenofovir disoproxil fumarate.
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