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HILIC B柱-HPLC法测定注射用门冬氨酸鸟氨酸的有关物质
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| 篇名： | HILIC B柱-HPLC法测定注射用门冬氨酸鸟氨酸的有关物质 |
| TITLE： | |
| 摘要： | 目的：建立测定注射用门冬氨酸鸟氨酸中有关物质的方法。方法：采用亲水作用色谱B柱-高效液相色谱（HILIC B柱-HPLC）法测定3批注射用门冬氨酸鸟氨酸的有关物质。色谱柱为ACE HILIC B，流动相为0.02 mol/L磷酸二氢钾缓冲液（pH 5.0）-乙腈（40 ∶ 60，V/V），检测波长为205 nm，流速为1.3 mL/min，柱温为30 ℃。对样品进行酸、碱、光、热、氧化破坏性试验，并将建立的方法与2015年版《中国药典》方法比较。结果：除光照破坏样品外，其余各条件破坏后样品与未破坏样品比较主峰面积均有所下降、杂质增多，各杂质间及与主成分峰间分离度均大于1.5；5个杂质马来酸、精氨酸、富马酸、门冬氨酸缩合物、3-氨基-2-哌啶酮及主成分门冬氨酸鸟氨酸的检测质量浓度线性范围分别为0.077 2～7.72、0.464～9.28、0.087 6～8.76、0.403～10.075、0.082 4～8.24、 1.613～80.7 μg/mL（r＝0.999 7～0.999 9），检测限分别为0.058、19、2.5、17、0.35、24 ng，定量限分别为0.19、63、8.3、56、1.2、80 ng。5个杂质的平均加样回收率为96.3％～102.1％（RSD＝0.4％～2.0％，n＝9）。3批样品中上述5个杂质的平均含量分别为0（未检出）、0、0.026％、0.011％、0.019％ ，与《中国药典》方法比较，测定结果相似，但后者进行2次系统适用性试验时各峰出峰顺序不一致。结论：建立的HILIC B柱-HPLC法简便、准确，耐用性和重现性优于《中国药典》方法，可以用于控制注射用门冬氨酸鸟氨酸的有关物质。 |
| ABSTRACT： | OBJECTIVE： To establish the method for the determination of related substances in Ornithine aspartate for injection. METHODS： A HILIC B column-HPLC method was used for the determination of related substances in 3 batches of Ornithine aspartate for injection. The determination was performed on ACE HILIC B column with mobile phase consisted of 0.02 mol/L monopotassium phosphate buffer solution （pH 5.0）-acetonitrile （40 ∶ 60， V/V） at the flow rate of 1.3 mL/min. The detection wavelength was set at 205 nm， and column temperature was 30 ℃. Acid， alkali， light， heat， oxidation forced degradation tests were carried out； established method was compared with the method stated in Chinese Pharmacopeia of 2015 edition. RESULTS： Except for light-destroyed samples， compared with undestroyed samples， main peak area of samples destroyed by other conditions was decreased certainly； the impurity was increased； the separation of impurities with main component peaks was higher than 1.5. The linear range of 5 impurities that maleic acid， arginine， fumaric acid， aspartic acid condensate， 3-mino-2-piperidone and main component ornithine aspartate were 0.077 2-7.72， 0.464-9.28，0.087 6-8.76，0.403- 10.075，0.082 4-8.24， 1.613-80.7 μg/mL （r＝0.999 7-0.999 9）， respectively. The limits of detection were 0.058， 19， 2.5， 17， 0.35 and 24 ng， respectively； the limits of quantitation were 0.19， 63， 8.3， 56， 1.2， 80 ng， respectively. The average recoveries of 5 impurities were 96.3％-102.1％ （RSD＝0.4％-2.0％，n＝9）. Average contents of 5 impurities in 3 batches of samples were 0 （not detected）， 0， 0.026％， 0.011％， 0.019％， respectively. Compared with the method of Chinese Pharmacopeia， established method obtained similar results， but the peak order of each peak was not consistent in 2 times of system suitability tests. CONCLUSIONS： Established HILIC B column- HPLC method is simple and accurate. It is better than the method stated in Chinese Pharmacopeia in durability and reproducibility. It can be used for controlling relevant substance in Ornithine aspartate for injection. |
| 期刊： | 2018年第29卷第19期 |
| 作者： | 胡兵，单晓芸，陈蔚江 |
| AUTHORS： | HU Bing，SHAN Xiaoyun，CHEN Weijiang |
| 关键字： | HILIC B柱-HPLC法；注射用门冬氨酸鸟氨酸；有关物质；破坏性试验 |
| KEYWORDS： | HILIC B column-HPLC method； Ornithine aspartate for injection； Related substance； Destructive test |
| 阅读数： | 566 次 |
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