【作者】 李伟；

【导师】 阚毓铭；

【作者基本信息】 南京中医药大学 ， 中药化学， 2001， 博士

【摘要】 从白术的乙醇提取物的乙酸乙酯萃取部分，分离得到十二个成分。根据波谱分析，鉴定出其成分分别为双白术内酯、苍术酮、白术内酯Ⅰ、白术内酯Ⅱ、白术内酯Ⅲ、蒲公英萜醇乙酸酯、β-香树脂醇乙酸酯、白术内酰胺、杜松脑、β-谷甾醇、γ-谷甾醇、尿苷。其中双白术内酯为一新化合物。 从化学角度对白术的炮制机理进行了研究，阐明了白术加工炮制中成分的变化过程。白术倍半萜类化合物在一定条件下可相互转化，苍术酮在空气中可氧化转变成白术内酯Ⅰ、Ⅲ及双白术内酯；白术内酯Ⅲ在盐酸-乙醇中加热可脱水生成白术内酯Ⅱ。 测定了白术炮制前后及不同炮制品中白术内酯Ⅰ、Ⅲ的含量。炒白术中白术内酯Ⅰ的含量明显提高，白术内酯Ⅲ的含量随着炒制程度的不同而成规律性差异。从理论上对炮制过程中成分的变化进行了探讨。 从白术的水提取液分离得到两种多糖PSAM-1和PSAM-2。并用HPLC法和¹³C-NMR等方法分别阐明多糖的化学结构。结果表明，多糖PSAM-1和PSAM-2均为杂多糖，平均分子量分别为1.36×10⁵、1.04×10⁵，PSAM-1由半乳糖、鼠李糖、阿拉伯糖、甘露糖组成，PSAM-2由木糖、阿拉伯糖、半乳糖组成。 采用淀粉酶比色测量法，进行了白术的水煎液、醇提液、白术挥发油及白术内酯Ⅰ、白术内酯Ⅲ对唾液淀粉酶活性影响的试验，结果表明，白术水煎液能明显增加酶的活性，白术醇提液及白术内酯Ⅰ对酶活性也有增强作用，而白术挥发油及白术内酯Ⅲ却抑制酶的活性 采用家兔外翻肠套法研究白术化学成分对小肠吸收营养物质的影响，实验结果表明，白术内酯Ⅰ能促进小肠对葡萄糖、Vitamin B6的 白术的有效物质及质量研究 论文掖要 吸收。而白术内酯＊无显著性的影响。 白术内酯1能桔抗乙酞胆碱引起的家兔离体肠管的痉挛，其量效曲 线符合非竟争桔抗剂特征，减活指数 PD厂力．14。白术内酯＊对离体肠 管则无明显作用。 研究了白术内酯1在家兔体内的药代动力学。用HPLC法测定生物 样品中白术内酯 1的浓度。家兔h白术内酯 IZ．5～10lug·kg－‘时的时 量曲线属二室模型。本品自家兔尿、粪的排出量很少。白术内酯1在家 兔体内吸收快、消除快、蛋白结合率高，主要分布在脑、心、肺、胆。 肾、小肠、肌肉等组织。 采用高效液相色谱法，对白术及苍术的醇－水提取物进行HPLC分析， 寻找白术区别于茅苍术和北苍术的特征性成分。白术样品有白术内酯1 和白术内酯m色谱峰，而茅苍术和北苍术样品都不明显。白术内酯1和 白术内酯m为白术区别于茅苍术和北苍术的特征性成分，可用HPLC法进 行区别。 采用薄层层析法和高效液相色谱法以白术内酯1、白术内酯＊为指 标成分，对白术的定性鉴别方法进行研究。两种方法均可用于白术的定 性鉴别。由于簿层层析法方法较为简便，故拟采用薄层层析方法。 采用反相高效液相色谱法，对白术中白术内酯1、11、Ill进行HPLC 分析，测定了25种不同白术样品中白术内酯的含量，平均加样回收率为 白术内酯1：98．4％，肪0为0．87％：白术内酯11：99．8％，RSD为1．2“ 白 术内酯＊：98．3兄RSD为1．l兄本法简单、灵敏、结果可靠，可作为白术 质量控制的定量方法。 考察白术指标成分的提取工艺，确定了标准物质的制备方法。 采用高效液相色谱法，建立了中成药香砂养胃丸中白术的定量测定 方法。采用m8柱（4．6x150m，10卜m），甲醇：水（6o：40）为流动相， 紫外检测波长220n，该方法线性良好，平均回收率为99．52％，RSD为 5 白术的有效物质及质且研究 论文箔要 1．7％。 提出了白术的质量标准修订草案，确定了以白术内酯1作为指标成 分，在现有中国药典（2000年版）的基础上增加了含量测定项，对原来 的定性鉴别项进行了修改，将原来所采用的定性指标成分苍术酮改为能 代表白术主要药效、且性质较为稳定的有效成分白术内酯I。更多还原

【Abstract】 The ethanol extract from the rhizoma Atractylodis macrocephalae was separated by column chromatography. Twelve compounds were isolated and were identified by spectra as biatractylenolide, atractylone, atractylenolide I, atractylenolide II, atractylenolide Ill, taraxeryl acetate , aniyrin acetate, atractylenolactam, junipercomphor3 P -sitosterol, i?-spinasterol, and uridine. The biatractylenolide is a new compound. The mechanism of processing was researched. Chemical component conversion during process was explained. Sesquiterpenes from Atracylodes macrocephala were researched. Atractylone can be oxidized to atractylenolide I and Ill in air: atractylenolide III can be converted to atractylenolide II in hydrochloride-ethanol. The contents of atractylenolide I and Ill both in raw and fried Atractylodes macrocephala were determined. The contents of atractylenolide I are noticeably increase after fried. The contents of atractylenolide III are different depend on the fry extent. The effects on starch enzyme activity of water extract, ethanol extract, essential oil, atractylenolide I and Lii from Atractylodes macrocephala were investigated by colorimetric analysis. Water extract can obviously increase the starch enzyme activity. Ethanol extract and atractylenolide I can also increase the enzyme activity. Oppositely, essential oil and atractylenolide III can inhibit the enzyme activity. The component’s effect on absorption of small intestine to nutritional materials was also investigated by reversed small intestine. Atractylenolide I can promote the absorption of glucose and Vitamin B6 in small intestine. 7 Atractylenolidelll didn’t show the activity apparently. Atractylenolide I can inhibit the spasm of rabbit intestine induced by acetylcholine. The amount-effect curve indicates the character of non- competitive. The decrease index pD2?~5.l4. AtractylenolideLll showed no activity. The pharmacokinetic character of atractylenolide I was investigated in rabbits. The contents of atractylenolide I in biological materials were determined by high-performance liquid chromatography. Plasma disposition followed a two-compartment model for atractylenolide 1 after an i.v. dose 2.5?10mg kg? Unchanged atractylenolide I rarely excreted via urine, feces and bile. Atractylenolide I was absorbed and eliminated rapidly. It distributed widely in brain, heart, lung, bile, kidney, small intestine and muscle .The protein binding was found to be high. Ethanol-water extracts from the rhizome of Atraciylodes macrocephala. Atractylodes lancea and Atractylodes chinensis were analyzed by high- performance liquid chromatography. Characteristic components distinguish Atractylodes macrocephala from Atractylodes lancea and Atractylodes chinensis were discovered. Atractylenolide I and atractylenolide 1171 were found in Atractylodes macrocephala, but not exist evidently in Atractylodes Iancea and Atractylodes chinensis. The qualitative controlling methods were studied by both thin-layer chromatography and high-performance liquid chromatography, with the atractylenolide I and atractylenolide 111 as the check samples. Both of the methods were available to qualitative analyses of Atractylodes macrocephala. The thin-layer chromatography method is selected because it is simpler than high-performance li更多还原