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| HPLC柱前衍生法测定舒血宁注射液中四种氨酸的含量 |
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陈莹1, 李晋1, 曹君2, 何俊1, 关秀伟3, 张纲4, 李志刚5, 常艳旭1
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1.天津中医药大学, 天津市现代中药重点实验室, 天津 300193;2.杭州师范大学材料与化学化工学院, 杭州 310036;3.河北神威药业有限公司, 廊坊 065200;4.河北省中药注射液工程技术研究中心, 廊坊 065200;5.中药注射剂新药开发技术国家地方联合工程实验室, 廊坊 065200
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| 摘要: |
| [目的] 建立舒血宁注射液中4种氨基酸（天门冬氨酸、苏氨酸、丙氨酸、甲硫氨酸）的高效液相色谱（HPLC）柱前衍生化法，为舒血宁注射液的质量控制提供方法。[方法] 以异硫氰酸苯酯（PITC）为柱前衍生化试剂，采用C18色谱柱，乙腈-水（5：1）-乙酸铵缓冲溶液（pH 6.5）为流动相，梯度洗脱，检测波长为254 nm，测定舒血宁注射液中天门冬氨酸、苏氨酸、丙氨酸、甲硫氨酸的含量。[结果] 4种氨基酸的分离及线性关系良好，精密度，重复性，稳定性RSD均都小于5%，平均回收率在95.6%~98.9%之间且RSD小于5%。舒血宁注射液中4种氨基酸总含量为1738.47μg/mL。其中甲硫氨酸含量最高，丙氨酸的含量最低。[结论] 本方法简便、准确、可靠，适用于舒血宁注射液中氨基酸含量的测定。 |
| 关键词: 舒血宁注射液 柱前衍生 天门冬氨酸 苏氨酸 丙氨酸 甲硫氨酸 |
| DOI：10.11656/j.issn.1673-9043.2017.04.15 |
| 分类号:R284 |
| 基金项目:国家重大新药创制项目（2014ZX09201022-004）；国家自然科学基金面上项目（81374050）。 |
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| Determination of four amino acids in Shuxuening injection by HPLC coupled with precolumn derivatization |
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CHEN Ying1, LI Jin1, CAO Jun2, HE Jun1, GUAN Xiu-wei3, ZHANG Gang4, LI Zhi-gang5, CHANG Yan-xu1
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1.Tianjin State Key Laboratory of Modern Chinese Medicine, Tianjin University of Traditional Chinese Medicine, Tianjin, 300193, China;2.College of Material Chemistry and Chemical Engineering, Hangzhou Normal University, Hangzhou 310036, China;3.Hebei Shineway Pharmaceutical Co., Ltd., Langfang 065200, China;4.Hebei Province Engineering Research Center for TCM Injection, Langfang 065200, China;5.Chinese medicine injection new drug development technology national local joint engineering laboratory, Langfang 065200, China
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| Abstract: |
| [Objective] To establish a HPLC method for determining 4 amino acids (aspartate, threonine, alanine and methionine) in Shuxuening injection.[Methods] HPLC analysis was performed after derivatization by using phenyl isothiocyanate (PITC) as a derivative reagent. Aspartate, threonine, alanine and methionine in Shuxuening injection were analyzed on C18 column with gradient elution of acetonitrile-water (5:1) and sodium acetate buffer solution (pH=6.5). The detection wavelength was at 254 nm.[Results] Separation and the linear relationships of 4 amino acids were good. All RSDs of precision, repeatability and stability were less than 5%. The sample recoveries were between 95% and 98%, with RSD less than 5%. The total content of four amino acids in Shuxuening injection was 1 738.47 μg/mL. The content of methionine was the highest in Shuxuening injection, while the content of alanine was the lowest.[Conclusion] The accurate and simple method was reliably applied to determine content of four amino acids in Shuxuening injection which could provide a scientific tool for the quality control of Shuxuening injection. |
| Key words: Shuxuening injection precolumn derivatization aspartic acid threonine alanine methionine |
