黄柏炮制原理及质量标准研究

【作者】 祁东利；

【导师】 贾天柱；

【作者基本信息】 辽宁中医药大学 ， 中药学， 2010， 硕士

【摘要】 目的:黄柏为芸香科植物黄皮树Phellodendron chinense Schneid.的干燥树皮,具有清热燥湿,泻火除蒸,解毒疗疮之效。盐黄柏为主要炮制品,临床上主要用于滋肾阴,泻相火。但是黄柏盐炙工艺参数不完善,本研究旨在优选黄柏盐炙工艺,分析炮制后化学成分变化,比较生制品滋肾阴作用,解析炮制原理,制定黄柏及盐黄柏质量标准。材料:黄柏丝、盐酸小檗碱、盐酸小檗红碱、盐酸黄柏碱方法:1.黄柏盐炙工艺研究通过单因素研究,选择炒制温度、炒制时间、加盐量和闷润时间为考察因素,以盐酸小檗碱和盐酸小檗红碱含量为指标,采用正交设计优选出黄柏盐炙工艺。以优选的工艺为基础,结合生产实际条件,炒制三个产地10批黄柏,确定黄柏中试盐炙工艺。2.黄柏盐炙前后化学成分变化研究通过薄层色谱和高效液相色谱法,比较黄柏盐炙前后化学成分变化情况。3.黄柏盐炙前后药理作用采用甲状腺素法造“甲亢肾阴虚症”大鼠模型,分别灌胃给于大鼠黄柏生品及盐炙品连续三周,测定血清中FT3、FT4含量、尿17--羟皮质类固醇含量、心率、红细胞膜Na+-K+-ATP酶活性,研究黄柏及其炮制品对神经内分泌系统的影响,比较黄柏炮制前后的滋阴作用情况;以干酵母致大鼠实热模型,观察黄柏生品和盐炙品对大鼠体温升高的抑制作用,比较黄柏生制品清实热的作用情况。4.黄柏及盐黄柏质量标准研究以盐酸小檗碱、盐酸小檗红碱和盐酸黄柏碱为指标,研究了黄柏和盐黄柏的质量标准。对十批不同产地黄柏和盐黄柏分别进行杂质、水分、总灰分、酸不溶性灰分、浸出物等方面的测定,制定了黄柏和盐黄柏质量标准。结果:1.确定黄柏盐炙最佳工艺:每100g黄柏加入盐2g,闷润1hr,在150～160℃条件下炒8分钟。以药材量的30%的水溶解盐;中试盐炙工艺:每100kg药材加入2kg盐,以盐水闷润,至药透汤尽后,置炒药机内在150℃-160℃炒制5分钟,用15L水溶解盐,炮炙耗率<4%。2.黄柏烘制后,盐酸小檗碱部分转化为盐酸小檗红碱,盐酸小檗红碱含量先升高,在180℃60min时其含量最高,达到1.86%,而后降低;黄柏烘制品和盐炙品中盐酸黄柏碱的含量均高于生品。3.黄柏生品及盐炙品能降低肾阴虚大鼠血清中FT3、FT4含量、心率和血液红细胞膜Na+-K+-ATP酶活性,盐炙品高剂量能降低大鼠尿17--羟皮质类固醇含量,二者具有滋肾阴作用,其中盐炙品作用强于生品;黄柏生品低剂量能够显著抑制大鼠的体温升高,具有良好的清热泻火作用,而盐炙品作用不明显。4.盐酸小檗碱、盐酸小檗红碱和盐酸黄柏碱的方法学考察中各项均符合有关规定。按干燥品计算,暂定黄柏中盐酸小檗碱含量不低于3.00%,盐酸黄柏碱含量不低于0.41%;盐黄柏中盐酸小檗碱含量不低于3.00%,盐酸小檗红碱含量不低于0.08%,盐酸黄柏碱含量不低于0.38%。结论:1.优选的盐炙黄柏最佳炮制工艺经过中试放大实验,其结果与初试结果基本一致,证明盐炙黄柏的炮制方法稳定可行。2.黄柏盐炙后,其成分发生了质变和量变,盐酸小檗碱部分转化为盐酸小檗红碱,盐酸黄柏碱的含量增加。这些成分变化为黄柏盐炙原理提供了重要依据。3.黄柏生品和盐炙品均具有滋肾阴的作用,且盐炙品作用强于生品,证实了黄柏盐制后引药入肾,滋肾阴作用增强的理论。4.黄柏生品和盐炙品均具有清实热的作用,且生品作用强于盐炙品,表明黄柏盐炙后,缓和了寒性,提示临床用于清实热时以生黄柏为宜。5.通过对不同产地黄柏及其盐炙品的杂质、水分、总灰分、浸出物和含量等的测定,所制定的黄柏和盐黄柏的质量标准稳定可行,并可用于评价和控制生、制黄柏的质量。更多还原

【Abstract】 Purpose:Cortex Phellodendri Chinensis is the dry bark of Phellodendron chinense Schneid.,which was commonly used to purge fire for removing toxin and eliminiate heat for drying moistenning. Cortex Phellodendri Chinensis with saltwater ,which is always applied to nourish Shen Yin in clinic ,is the major and popular processed product now,But its detail processing technology is not very clear.So the purpose of this study is to optimize the processing technology,research the changes of constituents,compare the function of nourishing Shen Yin before and after processing,establish the quality standard of Cortex Phellodendri Chinense and Cortex Phellodendron Chinensis with salt water,and clarify the principle of Cortex Phellodendri Chinensis processed with saltwater.Material:Cortex Phellodendri Chinensis、Berberine hydrochloride、Berberrubine hydrochloride、Phellodendrine hydrochlorideMethod:1.The content variation of Berberine hydrochloride and Berberrubine hydrochloride were selected as quality index,the influencing factors such as processing technology of processing temperature,processing time,the weight of salt and soaking time were optimized by L9(34) orthogonal design experiment.Based on this,industrial technology with salt water was determined according to quality of 10 piece of processed products.2. Compare the constituents between the crude and the processed product by TLC and HPLC.3. By intragastricing the rat mould of“hyperthyreosis”and Shen Yin deficiency symptoms”with the crude samples and the processed samples separately for three weeks,the content of FT3 ,FT4 in blood serum、17-OHCS in urine、heart rate and the activity of Na+-K+-ATPase were determined in order to compare the function of nourishing Yin before and after processing. The effect of the Cortex Phellodendri Chinensis and its processing product on the high temperature of mouse caused by yeast was test.4.Serving berberine hydrochloride、berberrubine hydrochloride and phellodendrine hydrochloride as index, the quality criteria of Cortex Phellodendri Chinensis and its processed product was established. The impurity,moisture content,ash content and extractive of the Cortex Phellodendri Chinensis and its processed product of ten habitats were determined.Result:1.Through single factor experiment and L9(34) orthogonal design,the optimum processing technology was set as follow:per 100 kg Cortex Phellodendri Chinensis used the salt 2 kg,solved by 30% of water of the medicinal materials.soaking 1 hour,frying 8 min at the temperature of 150～160℃;and industrial technology was set as follow: per 100 kg Cortex Phellodendri Chinensis used the salt 2 kg,solved by 15% of water of the medicinal materials.soaking 1 hour,frying 5 min at the temperature of 150～160℃.2.Part of berberine hydrochloride became berberrubine hydrochloride in processed products,and the the content of berberrubine hydrochloride increased at the beginning,the peak was 1.86% at the condition of 180℃and 60min,at last it went down.The study also showed that the content of Phellodendrine hydrochloride both in the product with saltwater and in the dried product was more than that of the crude product.3.The crude Cortex Phellodendri Chinensis and the processed products could reduce the content of FT3, FT4 in serum ,decrease heart rate and the activity of Na+-K+-ATPase,and high dose of the processed product could lower 17-hydroxy corticosteroid in urine significantly.both of them had the effect of nourish Shen Yin,and the product with salt water was powerful than the crude product.The low dose of the crude Cortex Phellodendri Chinensis could inhibited significantly the augmentation of mouse’temperature,and the processed worked insignificantly.4.The item in the methodology inspection of berberine hydrochloride、berberrubine hydrochloride、phellodendrine hydrochloride were qualified. The content of of berberine hydrochloride and phellodendrine hydrochloride in the Cortex Phellodendri Chinensis was tentatively fixed more than 3.00% and 0.41% respectively;The content of berberine hydrochloride、berberrubine hydrochloride and phellodendrine hydrochloride in the produnct with saltwater was more than 3.00%,0.08% and 0.38% respectively. Conclusion:1.The optimum processing technology of Cortex Phellodendri Chinensis with saltwater carried out in the amplification pilot,and was proved stable and feasible.2.Some qualitative and quantitative changes had taken placed in a group of constituents of alkaloids in Cortex Phellodendri Chinensis after processing.The changes was important to process theory of Cortex Phellodendri Chinensis with saltwater.3. Cortex Phellodendri Chinensis and the processed product with saltwater had function of nourish Shen Yin,and the processed product with saltwater was stranger than the crude product,which proved that the process with saltwater could bring drug into Shen Jing,and Strengthen the efficacy of nourish Shen Yin.4. Cortex Phellodendri Chinensis and the processed product with saltwater had function of eliminiating interior heat,and the crude product was better than the processed product with saltwater,which proved that the process with saltwater could moderate the coldness of Cortex Phellodendri Chinensis,and suggested that the crude product could be proper to apply in eliminiating interior heat.5. The impurity,moisture content,ash content and extractive of Cortex Phellodendri Chinensis and the processed example with saltwater of ten habitats were determined and the quality criteria of Cortex Phellodendri Chinensis and its processed product was stable and feasible,which could be used to evaluate and control their quality.更多还原