睡莲花总黄酮制备工艺及其质量标准研究

发布时间：2018-08-25 08:43

【摘要】：睡莲花Nymphaea candida Presl,维吾尔医称为“内鲁帕尔”,是雪白睡莲的干燥花蕾,该药材具有清热解毒、益心护脑、镇静安神等功效,在维医临床中主要用于热症引起的头疼、热感咳嗽及小儿急、慢惊风等病症的治疗。在前期研究基础上,本文对睡莲花总黄酮有效部位进行了以下几方面的研究。(1)通过高速逆流色谱对睡莲花标识性成分进行了分离纯化,采用乙酸乙酯-甲醇-水=(4:1:5 v/v)和乙酸乙酯-正丁醇-水=(4:1:5 v/v)作为溶剂体系,通过两步分离纯化得到了异槲皮苷、紫云英苷、isostrictiniin和烟花苷,它们的纯度分别为73.53%、92.42%、82.36%和85.65%。(2)以烟花苷、紫云英苷含量为考察指标,采用单因素考察结合正交试验优选出睡莲花总黄酮的最佳提取工艺为:提取溶剂选为70%的乙醇,料液比选为1:10、回流提取2次,每次提取时间为1.0 h。(3)以烟花苷、紫云英苷含量为考察指标,采用单因素考察优选出了睡莲花总黄酮的最佳纯化工艺:大孔树脂最佳上样浓度为烟花苷0.3220 mg/L、紫云英苷0.0865 mg/L,5BV 30%乙醇除杂,5 BV 50%乙醇洗脱;大孔树脂初步纯化后,再用聚酰胺吸附树脂进行富集纯化,其工艺条件为:样品与聚酰胺的比例为1:8,10 BV水除杂,5 BV 70%乙醇洗脱。(4)建立了睡莲花总黄酮的理化鉴别、薄层色谱鉴别方法;依据《中国药典》2015版第四部,测定了睡莲花总黄酮的水分、炽灼残渣、重金属和砷盐,初步限定含水分不得超过7.0%,炽灼残渣不得过4.0%,重金属不得过百万分之二十,砷盐不得过百万分之零点五。通过高温、高湿和强光等影响因素试验对睡莲花总黄酮进行初步稳定性研究,结果表明睡莲花总黄酮外观、色泽及总黄酮标示性成分无明显影响,性质稳定。建立了HPLC法测定睡莲花总黄酮标识性成分含量测定的方法。建立了分光光度法测定睡莲花总黄酮含量的方法。
[Abstract]:Water lily flower Nymphaea candida Presl, Uygur medicine is called "Nerupar", is the dry flower bud of white water lily. It has the functions of clearing heat and detoxifying, benefiting heart and protecting brain, calming and calming the mind, etc. It is mainly used for headache caused by hyperthermia in Uygur medicine. The treatment of fever cough and acute and slow shock in children. On the basis of previous studies, the effective components of total flavonoids in water lily flower were studied in the following aspects. (1) the identifiable components of water lily flower were separated and purified by high speed countercurrent chromatography. Using ethyl acetate, methanol-water = (4:1:5 v / v) and ethyl acetate / n-butanol-water = (4:1:5 v / v) as solvent system, isostrictiniin and pyroginoside were separated and purified by two steps. Their purity were 73.53% 92.4282.36% and 85.65% respectively. (2) the purity of isostrictiniin was 73.53%. The optimum extraction technology of total flavonoids of water lily flower was selected by single factor investigation combined with orthogonal test. The optimum extraction process was as follows: the solvent was selected as 70% ethanol, the ratio of material to liquid was 1: 10, and the reflux extraction was 2 times. The extraction time was 1.0 h. (3) the contents of fireworks and porphyrin were used as the index. The optimum purification process of total flavonoids from water lily flower was investigated by single factor. The best concentration of macroporous resin was 0.3220 mg/L, 0.0865 mg/L,5BV 30% ethanol, 5 BV 50% ethanol elution, and after the primary purification of macroporous resin, the optimum concentration of macroporous resin was 0.3220 mg/L,5BV, 30% ethanol and 50% ethanol, respectively. Then the polyamide adsorbent resin was used for enrichment and purification. The technological conditions were as follows: the ratio of sample to polyamide was 1: 8 ~ (10) BV water removal was 5 BV 70% ethanol elution. (4) Physicochemical identification and TLC identification of total flavonoids of water lily flower were established. According to the fourth part of the 2015 edition of the Chinese Pharmacopoeia, the water content, incandescent residue, heavy metal and arsenic salt of the total flavonoids of water lily flower were determined. The preliminary limit was that the moisture content should not exceed 7.0, the incandescent residue should not exceed 4.0, and the heavy metal should not exceed 20/1000000. Arsenic should not exceed 0.5/1000000. The effects of high temperature, high humidity and strong light on the stability of total flavonoids in water lily flower were studied. The results showed that the appearance, color and marked composition of total flavonoids in water lily flower were not significantly affected, but the properties were stable. A HPLC method for the determination of total flavonoids in water lily was established. A spectrophotometric method for the determination of total flavonoids in water lily flower was established.
【学位授予单位】：新疆大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TQ464

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