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光度法研究姜黄素与铁络合反应及液相色谱法研究生产中盐酸氯己定的质量控制

Study on the Curcumin’s Complex Reaction with Iron by UV-VIS and the Qulity Control of Chlorhexidine Hydrochloride in Production Process by HPLC

【作者】 屈英格

【导师】 程忠洲;

【作者基本信息】 西北大学 , 分析化学, 2010, 硕士

【摘要】 本论文共分4章,具体内容如下:第一章绪论,综述了紫外可见分光光度法、高效液相色谱法在药物分析中的应用及论文的研究背景。第二章用光度法研究姜黄素与铁(Ⅲ)络合反应,建立测定水中铁含量的方法。姜黄素是从姜黄属根茎中提取的天然酚类物质,具有抗氧化、抗癌、抗炎等多种药理活性,无毒,是理想的绿色离子显色剂。研究发现,姜黄素在较高浓度时,能自动聚合,与铁(Ⅲ)反应灵敏。摩尔吸收系数为3.86×104L·mo1-1·cm-1,比二氮杂菲等方法高约3倍。在此基础上,建立了测定水中铁(Ⅲ)含量的姜黄素光度法,平均回收率为101.7%。该方法操作简单,灵敏度高,选择性较好,可用于水中铁的测定。第三章用姜黄素光度法研究复方硫酸亚铁叶酸片中铁(Ⅱ)的测定方法。复方硫酸亚铁叶酸片是由硫酸亚铁、叶酸、干酵母、当归、黄芪、白术等组成的复方制剂,属抗贫血药。在前章研究基础上,建立了测定复方硫酸亚铁叶酸片中铁(Ⅱ)含量的姜黄素光度法,平均回收率为101.6%,相对标准偏差为1.7%。摩尔吸收系数为3.69×104L·mo1-1·cm-1,比该药质量标准中所用邻菲罗啉分光光度法高约3倍。该方法快速、准确、灵敏,可用于复方硫酸亚铁叶酸片的质量控制。第四章用HPLC法研究生产过程中盐酸氯己定的质量控制。经反复试验、筛选的色谱条件为:采用ODS柱(150 mm×4.6 mm,5μm),以甲醇:0.06 mol·L-1 KH2P04-0.07 mol·L-1H3P04(54:46,V/V)为流动相,检测波长240 nm,流速0.8 mL·min-1,柱温35℃。在此条件下,各组分峰形对称,分离效果理想。测得盐酸氯己定、反应物对氯苯胺的相关系数均为0.9999,平均回收率分别为101.1%,100.5%。该方法选择性好,灵敏度高,适于该药生产过程及日常质量控制。

【Abstract】 There are four parts in this thesis. Details are as follows:In the first chapter, the applications of Ultraviolet-Visible Spectrophotometry and High Performance Liquid Chromatography in pharmaceutical analysis are reviewed, and the research background is introduced.In the second chapter, curcumin’s complex reaction with Iron was studied, and a method was established for the determination of Iron (Ⅲ) in tap water by UV-VIS.Curcumin is a natural phenolic substance contained in the rhizome of Curcuma longa. It has been reported to possess a variety of pharmacological activities such as antioxidant, anti-cancer, anti-inflammatory, no toxicity. It is an ideal "green" ions color reagent. At the higher concentration, polymerized curcumin is more sensitive to complex with Fe (Ⅲ). The molar absorptivity is 3.86×104 L·mol-1·cm-1, which is higher 3 times than Phenanthroline spectrophotometry. The proposed UV-VIS method was established for the determination of Iron (Ⅲ) in tap water. The average recovery of Iron (Ⅲ) was 101.7%. It is simple, sensitive, selective, and suitable for the determination of Iron (Ⅲ) in tap water.In the third chapter, a method was established for the determination of Iron(Ⅱ) in Compound Ferrous Sulfate and Folic Acid Tablets by curcumin spectrophotometry.Compound Ferrous Sulfate and Folic Acid Tablets are the compound preparation composed of Ferrous Sulfate, folic acid, dry yeast, Angelica, Astragalus, Largehead Atractylode, et al.. It is a antianemic agent. Based on the previous chapter, a method was established for the determination of Iron (Ⅱ) in the tablets by curcumin spectrophotometry. The average recovery and RSD of Iron (Ⅱ) were 101.6% and 1.7%, respectively. The molar absorptivity is 3.69×104 L·mol-1·cm-1, which is higher 3 times than Phenanthroline spectrophotometry. The method is convenient, accurate, sensitive, and suitable for the quality control of Compound Ferrous Sulfate and Folic Acid Tablets.In the forth chapter, the quality control of Chlorhexidine Hydrochloride in the production process was studied by HPLC.The analysis was carried out with ODS column (150 mm×4.6 mm,5μm), using methanol:0.06 mol·L-1 KH2PO4-0.07 mol·L-1 H3PO4 (54:46, V/V) as the mobile phase. The flow rate was 0.8 mL·min-1, the detection was set at 240 nm and the column temperature was maintained at 35℃. Under this conditions, each compound’s peak shape was symmetrical and the separation was good. The correlation coefficient of Chlorhexidine Hydrochloride and p-Chloroaniline were 0.9999, the average recoveries were 101.1% and 100.5%, respectively. The proposed method has good selectivity and sensitivity, and can be used for the quality control of Chlorhexidine Hydrochloride in the production process and daily.

  • 【网络出版投稿人】 西北大学
  • 【网络出版年期】2010年 09期
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