黑米花青素片剂的制备工艺及质量标准研究

发布时间：2017-12-28 06:14

本文关键词：黑米花青素片剂的制备工艺及质量标准研究　出处：《吉林大学》2017年硕士论文　论文类型：学位论文

【摘要】：随着社会的进步和经济的发展,人们对自身健康日益关注,用食品调节人体机能已成为民众的健身手段。花青素是自然界中广泛存在于植物中的水溶性天然色素,其抗氧化保健功能已被广泛研究,但目前摄入花青素的方式仍为食补,关于其制剂的研究非常少,限制了其应用,因此,研究花青素制剂具有广阔的市场前景。黑米中含有以矢车菊素-3-O-葡萄糖苷为主成分的花青素。本文以黑米花青素为原料,开发黑米花青素片剂,对其制备工艺及质量标准进行研究。本文通过研究得出结果如下:(一)原料性质:高湿条件及强光照射条件对黑米花青素稳定性影响较大,高温条件对其稳定性影响较小,黑米花青素在室温下分解10%所需的时间为210天。Fe~(2+)、Fe~(3+)、Cu~(2+)均使其含量明显下降,其中Fe~(3+)影响最大,Mg~(2+)有增加稳定性的作用。酸性条件有利于黑米花青素的稳定,且溶液pH值越低,黑米花青素越稳定。原料本身流动性很差(休止角α=61.07°,松密度ρ松=0.235,振实密度ρ实=0.407,压缩度=42.26%),属于“有引湿性”。(二)制剂工艺:黑米花青素与稀释剂的最佳配比为1:1,稀释剂中淀粉与糊精的最佳配比为1:1.5,崩解剂交联聚乙烯比咯烷酮(PVPP)的最佳用量为2%,润湿剂中乙醇的最佳浓度为75%。黑米花青素成型制备工艺如下:黑米花青素与各辅料分别过100目尼龙药筛,按处方量称重,将黑米花青素与稀释剂及1/2崩解剂混合均匀,将酒石酸分散于适量润湿剂中,制软材,过20目尼龙药筛制粒,颗粒在45℃条件下干燥,干燥后过20目筛整粒,细粉与硬脂酸镁及另外1/2崩解剂混合均匀后再与颗粒混匀,压片。按成型处方及工艺制备的黑米花青素片剂,经质量检查符合药典要求,处方及制备工艺合理。(三)质量标准研究:本品为深紫色凸面圆形片剂,大小均匀、色泽一致,表面完整光洁。以矢车菊素-3-O-葡萄糖苷为对照品进行鉴别,鉴别方法为高效液相法。3批黑米花青素片剂各项质量检查均合格。采用高效液相法测定制剂中矢车菊素-3-O-葡萄糖苷的含量,经考察,该方法理论塔板数N=3947,重复性好(RSD=1.32%),灵敏度高(检出限为0.2μg/mL,定量限为1μg/mL。),峰无前延或拖尾现象(拖尾因子T=0.97),分离度R=2.411.5,完全分离,方法专属性强,精密度高(日内精密度RSD=0.37%,日间精密度RSD=0.63%),准确度可满足复杂成分的检测要求(加样回收率=78.89%),且12小时内稳定(RSD=0.76%),方法可靠,适用于本制剂中矢车菊素-3-O-葡萄糖苷的含量测定。除此之外,采用色价法测定制剂中总黑米花青素的含量,方法精密度高(日内精密度RSD=0.87%,日间精密度RSD=1.19%),准确度可满足检测要求(加样回收率=81.71%),且12小时内稳定(RSD=1.29%),方法可靠,适用于本制剂中总花青素含量的测定。(四)体外抗氧化活性测定:黑米花青素原料及其制剂均表现出较强的体外自由基清除能力及抗氧化还原能力。制剂过程对黑米花青素的抗氧化活性未有大的影响。(五)片剂初步稳定性:影响因素试验中,温度对黑米花青素片剂稳定性影响最小,室温下分解10%所需的时间为427天。高湿条件及强光照射条件下,黑米花青素片剂稳定性相对较低,在加速试验条件下,3个批次黑米花青素片剂的稳定性随时间的增加略有降低。综上所述,黑米花青素片剂的制备工艺切实可行,质量控制方法科学合理,准确可行。
[Abstract]:With the progress of the society and the development of the economy, people are increasingly concerned about their own health. The use of food to regulate human functions has become a means of fitness for the people. Anthocyanins are widely present in nature in plants in the water soluble natural pigment, antioxidant health function has been extensively studied, but there is still intake from Sibu, research on its preparation is very few, therefore, limit the application of anthocyanin preparation has broad market prospects. Black rice contains anthocyanins, which are mainly composed of -3-O- glucoside. In this paper, black rice anthocyanins are used as raw materials to develop black rice anthocyanin tablets. The preparation technology and quality standard of black rice are studied. In this paper, the following research results are as follows: (1) raw material properties: high humidity condition and strong light irradiation condition have great influence on the stability of anthocyanin in black rice. The influence of high temperature on its stability is relatively small. The time needed to decompose 10% of anthocyanins in black rice at room temperature is 210 days. The content of Fe~ (2+), Fe~ (3+) and Cu~ (2+) all decreased obviously, of which Fe~ (3+) had the greatest influence, and Mg~ (2+) had the effect of increasing stability. The acid condition is beneficial to the stability of black rice anthocyanin, and the lower the pH value of the solution, the more stable the black rice anthocyanin. The raw material itself illiquid (repose angle alpha =61.07 degrees, the density of pine pine =0.235, tap density is =0.407, compression degree =42.26%), is a "moisture". (two) preparation process: the best ratio of black rice anthocyanin and diluent is 1:1, the best ratio of starch to dextrin in diluent is 1:1.5, the best dosage of disintegrating agent crosslinked polyethylene, PVPP is 2%, and the best concentration of ethanol in wetting agent is 75%. The black rice anthocyanins forming preparation process are as follows: the black rice anthocyanins and other auxiliary material are 100 mesh nylon sieve, weighing according to the prescription, and will be the black rice anthocyanins diluent and disintegrating agent 1/2 mixed evenly, the tartaric acid dispersed in the amount of wetting agent, made of soft material, 20 mesh nylon sieve granulation, granule at 45 DEG C under the conditions of drying, drying after 20 mesh fine powder with whole grain, magnesium stearate and 1/2 disintegrating agent are mixed evenly and then with the particle mixing and tabletting. The black rice anthocyanin tablets prepared by the molding prescription and process are in accordance with the requirements of the Pharmacopoeia, and the formulation and preparation process are reasonable. (three) quality standard study: This product is a deep purple convex surface circular tablet with uniform size, uniform color and smooth surface. -3-O- glucoside was identified as a control product, and the identification method was high performance liquid phase method. The quality of the 3 batch of black rice anthocyanins were all qualified. The content of the -3-O- N=3947 glucoside in the preparation was determined by HPLC. The theoretical plate number is N=3947, repeatability is good (RSD=1.32%), and the sensitivity is high (the detection limit is 0.2 g/mL, and the limit of quantification is 1 g/mL. No delay before the peak), or smearing (trailing factor T=0.97), the degree of separation of R=2.411.5, completely separated. The method has high specificity and high precision (the precision of RSD=0.37%, the intra and inter day precision RSD=0.63%), accuracy can meet the detection requirements of complex components (recovery rate = 78.89%), and 12 hours stable (RSD=0.76%), the method is reliable and suitable for the determination of the preparation of cyanidin glucoside -3-O-. In addition, determination of total anthocyanins in black rice preparation by color value method, method of high precision (the precision of RSD=0.87%, the intra and inter day precision RSD=1.19%), accuracy can meet the requirements of detection (recovery =81.71%), and within 12 hours of stable (RSD=1.29%), the method is reliable and suitable for determination of the total anthocyanin content of the preparation. (four) determination of antioxidant activity in vitro: black rice anthocyanin material and its preparation all showed strong free radical scavenging ability in vitro and antioxidant reduction ability. The preparation process has no significant effect on the antioxidant activity of black rice anthocyanins. (five) the initial stability of the tablets: the influence of temperature on the stability of black rice anthocyanin tablets was the least, and the time required for decomposition of 10% at room temperature was 427 days. Under the condition of high humidity and strong light, the stability of black rice anthocyanin tablets was relatively low. Under accelerated test conditions, the stability of 3 batches of black rice anthocyanin tablets decreased slightly with time. To sum up, the preparation technology of black rice anthocyanin tablets is practical, the quality control method is scientific and reasonable, and it is accurate and feasible.
【学位授予单位】：吉林大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：R943

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