摘要
人参(Panax ginseng C.A.Mey.)为五加科人参属植物,是中国传统的名贵中药,具有滋补养气、活血化瘀、止咳平喘、延年益寿等功效。人参多糖是人参的重要活性成分之一,具有抗肿瘤、抗衰老、降血糖、降血脂和调节免疫等功能。
本论文以人参为原料,从鲜人参根中提取人参多糖(葡聚糖),以此为原料合成人参硫酸酯多糖,并对合成产物的结构进行了表征;建立了人参中19种有机氯农药的多残留分析方法。
1.采用水提醇沉法对鲜人参根中的人参多糖进行了提取研究,优选出人参多糖的最佳提取条件和提取方法;利用高效液相色谱测定人参多糖的平均分子量约为10,300;利用红外光谱法测定其分子结构为吡喃型α-D-葡聚糖。
2.本论文首次以人参多糖为原料,利用氯磺酸-吡啶法合成人参硫酸酯多糖。通过比较吡啶与氯磺酸体积比、反应温度和反应时间等反应条件,优选出人参硫酸酯多糖的最佳合成条件,得到硫取代度2.05的人参硫酸酯多糖。
3.利用高效液相色谱法、紫外光谱法和红外光谱法对人参硫酸酯多糖的结构进行了表征:高效液相色谱表明人参硫酸酯多糖有单一色谱峰,说明成分较均一;紫外光谱表明在250~275nm处有-SO_3特征吸收峰;红外光谱表明在1257cm~(-1)处有-OSO_3的S=O伸缩振动;826 cm~(-1)左右的吸收表明为C-O-S的伸缩振动特征吸收峰;说明合成产物有硫酯键。
4.利用核磁共振碳谱法对硫酸根的取代位置进行了测定。结果表明硫酸根优先取代C-6羟基上的氢,说明在此反应中,人参多糖的单糖残基上C-6羟基的活性大于C-2、C-3和C-4。
5.建立了人参中19种有机氯农药的多残留分析方法,该分析方法的准确度和精密度的测定结果均符合农药残留分析的要求。其中,19种有机氯农药的峰面积与其质量浓度均有良好的线性关系,相关系数均大于0.992,方法的最低检出限为1.5×10~(-13)-2.5×10~(-12)g,样品的加标平均回收率为75.7%-115.2%。
6.本论文所合成的人参硫酸酯多糖,具有成分均一、分子量较小和高硫取代度的特点,为可能具有高生物活性的抗艾滋病、抗肿瘤的药物研究提供样品。
7.本论文所建立的人参有机氯农药的多残留分析方法,可以为提高我国人参产品的质量,增强其在市场中的竞争能力,进一步同国际市场接轨,促进人参行业的发展和中药现代化,提供良好的检测技术手段。
Panax ginseng C.A.Mey. is a plant of Araliaceae. Ginseng with high reputation and expensive value is usurally regarded as one kind of Chinese traditional herb which has many medical effecets, such as keeping the halth in balance, making the blood more fresh, keeping the cough off earlier, and delaying the life period, etc. Extracted from panax ginseng, Polysaccharide, as one of the main active components, has various fuctions such as anti-tumor, anti-caducity, decreasing blood sugar and blood fat, and modulating immnity, etc.
The thesis introduces the Ginseng polysaccharides which are extracted from fresh root of ginseng and belongs to one kind of D-dextrans. A kind of sulfated polysaccharides was obtained and its struction was proved. A new method for analysis of nineteen organochlorine pesticide residues in Ginseng is proposed.
1. The best conditions and methods of extracting Ginseng polysaccharides are indentified through comparing the water extraction-ethanol deposition. The average molecular weight is about 10,300 of Ginseng polysaccharides by HPLC. The molecular structure is Pyran-typedα-D- dextrans by FT-IR.
2. Ginseng sulfated polysccharides was obtained from Ginseng polysaccharides with chlorosulfonic acid-pyridine in this paper first. The best conditions of synthesis through comparing the effects of different conditions such as vol.proportion of chlorosulfonic acid-pyridine, reactive temperature and reactive time. Replace degree of S is 2.05.
3. By means of HPLC, UV and FT-IR, the structure of ginseng sulfated polysccharides was proved. The HPLC chromatogram shows a single peak; the UV spectrum of Ginseng sulfated polysccharides shows the characteristic absorptions of sulfate ester bond at 250~275nm; the FT-IR spectrum of Ginseng sulfated polysccharides shows the characteristic absorptions of sulfate ester bond at 1257cm~(-1) and 826cm~(-1). These show that synthesis of the sulfate ester is made.
4. The ~(13)C NMR spectrum of Ginseng sulfated polysccharides shows that hydroxyl of C-6 is more active than those of C-2, C-3 and C-4.
5. The multiresidue analysis method of nineteen organochlorine pesticide were established which qualifies the precision and accuracy corresponds with requirement of the analysis of the pesticide residues. The good linearity were obtained for nineteen organochlorine pesticide with the average relative coefficient larger than 0.992. The minim detectable sample was1.5×10~(-13)~2.5×10~(-12) g, and the average recoveries range was from 75.7% to 115.2%.
6. In the thesis, Ginseng sulfated polysccharides synthesized include some characteristics of homogeneous component, lesser molecular weight, more replace degree of S, which provide the sample for the more biology-action of anti-AIDS and anti-tumour.
7. The multiresidue analysis method in the thesis may be applied in some fields widespreadly and provides good technoloy of supporting gensing quality improvement to increase the competitive capacity of International ginseng market, accelerate the development and modernazation of the profession of gensing with the advanced means of testing.
引文
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