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盐酸氨基葡萄糖片中5-HMF的含量测定及形成动力学研究
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| 篇名： | 盐酸氨基葡萄糖片中5-HMF的含量测定及形成动力学研究 |
| TITLE： | Content determination of 5-HMF in glucosamine hydrochloride tablets and formation kinetics study |
| 摘要： | 目的 建立测定盐酸氨基葡萄糖片中5-羟甲基糠醛（5-HMF）含量的方法，分析其含量变化规律及影响因素。方法采用高效液相色谱法对5-HMF进行定量测定，以Shim-packGISTC18-AQ为色谱柱，0.1%磷酸溶液-甲醇（90∶10，V/V）为流动相，柱温为30℃，检测波长为284nm，流速为1.0mL/min，进样量为20μL。通过不同温度反应动力学实验分析5-HMF含量与反应温度、反应时间的相关性，建立其形成动力学模型。结果5-HMF检测质量浓度的线性范围为0.057～5.698μg/mL（r＝0.9999）；检测限为5.70ng/mL，定量限为17.09ng/mL；精密度、重复性和稳定性（24h）试验的RSD均小于1.0%（n＝6）；加样回收率为99.38%～99.73%（RSD＝0.53%，n＝9）。8批样品含量为4.10～35.13μg/g。反应动力学实验数据拟合结果显示，随着反应温度升高、反应时间延长，样品中5-HMF含量越高。50、60、70、80℃下，5-HMF含量与反应时间均呈线性关系，符合零级动力学模型，反应速率常数分别为6.789、7.715、8.815、11.430。结论所建含量测定方法专属性强、灵敏度高、准确度好；反应温度和反应时间是影响盐酸氨基葡萄糖片中5-HMF形成的重要因素，其含量变化规律符合零级动力学模型。 |
| ABSTRACT： | OBJECTIVE To establish the method for the content determination of 5-hydroxymethylfurfural （5-HMF） in glucosamine hydrochloride tablets， and to analyze its regularity and influential factors. METHODS Quantitative analysis of 5-HMF was performed using high-performance liquid chromatography. The analysis was conducted on Shim-pack GIST C18-AQ column with mobile phase consisted of 0.1% phosphoric acid solution-methanol （90∶10， V/V） at the flow rate of 1.0 mL/min. The column temperature was 30 ℃， and detection wavelength was 284 nm. The injection volume was 20 μL. Reaction kinetics test of different temperatures was adopted to analyze the relationship of 5-HMF content with reaction temperature and reaction time， and utilized to build its formation kinetic model. RESULTS The linger range of 5-HMF was 0.057-5.698 μg/mL （r＝0.999 9）. The limits of detection and quantitation were 5.70 and 17.09 ng/mL； RSDs of precision， repeatability and stability （24 h） tests were all lower than 1.0% （n＝6）. The average recoveries ranged from 99.38% to 99.73%（RSD＝0.53%， n＝9）. The contents of the 5-HMF in 8 batches of samples ranged 4.10-35.13 μg/g. Results of data fitting in reaction kinetics test showed that the higher reaction temperature and the longer reaction time， the higher 5-HMF content in the sample. At 50， 60， 70 and 80 ℃ ， the relationship between the content of 5-HMF and the reaction time was linear， in accordance with a zero-order kinetic model. The reaction rate constants were 6.789， 7.715， 8.815 and 11.430， respectively. CONCLUSIONS The established method has strong specificity， high sensitivity， and good accuracy； the reaction temperature and reaction time are important influential factors for the formation of 5-HMF in glucosamine hydrochloride tables. The change rule of its content conforms to the zero-order kinetic model. |
| 期刊： | 2023年第34卷第08期 |
| 作者： | 倪东宇；王琼芬；张梦奇；李彬；石婧；徐虹；张帅 |
| AUTHORS： | NI Dongyu，WANG Qiongfen，ZHANG Mengqi，LI Bin，SHI Jing，XU Hong，ZHANG Shuai |
| 关键字： | 盐酸氨基葡萄糖片；5-羟甲基糠醛；高效液相色谱法；含量测定；形成动力学 |
| KEYWORDS： | glucosamine hydrochloride tables； 5-hydroxymethylfurfural； HPLC； content determination； formation kinetics |
| 阅读数： | 168 次 |
| 本月下载数： | 4 次 |
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