| 陈宇堃,蒋玉辉,梁蔚阳.HPLC法测定复方氨基酸（15）双肽（2） 注射液中有关物质的含量[J].中国药品标准,2019,20(1):25-30 |
| HPLC法测定复方氨基酸（15）双肽（2） 注射液中有关物质的含量 |
| Determination of Related Substances in Compound Amino Acid (15) and Dipeptides (2) Injection |
| 投稿时间：2018-07-17 修订日期：2019-01-15 |
| DOI： |
| 中文关键词: 复方氨基酸（15）双肽（2）注射液 HPLC 有关物质 环-（甘氨酰谷氨酰胺） 焦谷氨酸 环-（甘氨酰酪氨酸） |
| 英文关键词: Compound Amino Acid (15) and Dipeptides (2) Injection HPLC related substances cyclo-(Gly-Gln) pyroglutamicacid cyclo-(Gly-Tyr) |
| 基金项目:广东省医学科学技术研究基金项目（B2016121、B2018130）；广东省省级科技计划项目（2015A030402004） |
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| 中文摘要: |
| 目的：建立测定复方氨基酸（15）双肽（2）注射液中有关物质含量的高效液相色谱法。方法：采用Ultimate AQ-C18（250mm *4.6mm，5µm）色谱柱，以0.01mol?L-1磷酸氢二铵溶液（pH2.0）-甲醇（98：2）为流动相，流速为0.7mL?min-1，检测波长为205nm，进样量为50µL。结果：在选定的色谱条件下，环-（甘氨酰谷氨酰胺）峰、焦谷氨酸峰和环-（甘氨酰酪氨酸）峰与各自相邻色谱峰可以有效分离；环-（甘氨酰谷氨酰胺）、焦谷氨酸、环-（甘氨酰酪氨酸）分别在7.863～52.42µg?mL-1、5.256～35.04µg?mL-1、0.9393～6.262µg?mL-1的范围内线性关系良好（r=0.9999）；精密度试验的RSD值均小于0.2%；重复性试验的RSD值均小于2.0%；环-（甘氨酰谷氨酰胺）、焦谷氨酸和环-（甘氨酰酪氨酸）定量限分别为3.15、14.0和7.5ng，检测限分别为0.95、7.0和2.5ng；加样回收率分别为103.0、101.5和103.3%（n=9），RSD值分别为1.0%、0.9%和0.9%。结论：该方法专属性强，结果准确，可用于复方氨基酸（15）双肽（2）注射液中有关物质的测定，能有效的反应药品质量。 |
| 英文摘要: |
| Objective: To establish a HPLC method for determination of related substances in Compound Amino Acid (15) and Dipeptides (2) Injection.Methods: The test was performed on the column of Ultimate AQ-C18（250mm *4.6mm，5µm）. The mobile phase was 0.01mol?L-1 ammonium hydrogen phosphate buffer solution (pH2.0)-methanol (98:2) at a flow rate of 0.7mL?min-1.The detection wavelength was 205nm andthe injection volume was 50µL. Results: Under the selected HPLC conditions, the peak of cyclo-(Gly-Gln), pyroglutamic acid and cyclo-(Gly-Tyr) can be effectively separated from their adjacent chromatographic peaks. There were good linear relationship with r=0.9999 in the range of 7.863～52.42µg?mL-1、5.256～35.04µg?mL-1、0.9393～6.262µg?mL-1 for cyclo-(Gly-Gln), pyroglutamic acid and cyclo-(Gly-Tyr) respectively. The RSDs of the precision tests were not more than 0.2% and the RSDs of the stability test were not more than 2.0%. The limits of quantification of cyclo-(Gly-Gln), pyroglutamic acid and cyclo-(Gly-Tyr) was3.15、14.0 and 7.5ng respectively. The limits of detection of cyclo-(Gly-Gln), pyroglutamic acid and cyclo-(Gly-Tyr) was 0.95、7.0 and 2.5 ng respectively. The average recoveries were 103.0%、101.5% and 103.3%（n=9），RSDs of the average recoveries were 1.0%、0.9% and 0.9% respectively.Conclusion: The established method is reproducible and suitable for determination of the related substances inCompound Amino Acid (15) and Dipeptides (2) Injection. |
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