【作者】 贾存勤；

【导师】 李阳春； 屠鹏飞；

【作者基本信息】 甘肃农业大学 ， 草业科学， 2003， 硕士

【摘要】 大孔吸附树脂是一种具有大孔网状结构的高分子吸附剂，对水溶性化合物具有特殊的吸附作用，近年来大孔吸附树脂已经较为广泛地应用于中药及天然药物的分离和纯化当中。目前国产的商品大孔树脂大都含有一定量的有机残留物，造成了经大孔树脂纯化后的药品的不安全性。为了建立简便的大孔树脂有机残留物的检测方法和有效的大孔树脂处理方法，为科研和生产带来方便，我们进行了以下研究。 采用气相—质谱联用技术确定了九种大孔吸附树脂的有机残留物种类，其中甲苯、二乙苯和萘为九种大孔树脂所共有，其它苯系物如二甲苯、苯乙烯和二乙烯苯等也有检出，但含量不高；另外，在三种树脂中检出了多种烃类，其中癸烷、十一烷和十二烷的含量最高。 利用气相色谱法和紫外光谱法在研究树脂预处理方法时发现，溶剂和温度是树脂预处理过程中两个关键的因素。在一定温度下，大孔树脂经2倍树脂柱体积(2BV)的5％NaOH溶液和3～5BV有机溶剂浸泡、洗脱后，已基本干净。本方法工艺简单、环境污染小、溶剂用量少、预处理时间短。此外，我们发现，当洗脱液的紫外吸收值(λ=254nm)为0.2～0.4时，利用气相色谱法检测大孔树脂中的有机残留物已很少，这就说明紫外吸收值的大小可以在一定程度上反映有机残留物的多少。提示我们可以用紫外的方法监测树脂的有机残留物。 建立了气相色谱法检测大孔吸附树脂和药品中有机残留物的方法。本方法操作方便、检测灵敏，可以在同一根色谱柱上在短时间内测定所有需要检测的十种有机残留物的含量。 制定了药用大孔吸附树脂的质量标准：树脂以干重计，规定苯不得大于2ppm，甲苯、二甲苯、苯乙烯、二乙苯、二乙烯苯、萘、癸烷、十一烷和十二烷不得大于20ppm。 对于大孔树脂在中草药分离、纯化中的应用进行了研究。栀子和贯叶金丝桃的主要有效成分分别是桅子营、藏红花素及黄酮类化合物，利用大孔树脂纯化二者有效成分的研究还未见报道。我们研究了13种大孔吸附树脂对桅子中环烯迷菇普类化合物的吸附-胜能，其中吸附量较大的树脂型号是:HPDIOO、AB一8、SP825和SPZO7。树脂AB一8的分离度最好。同时建立了用树脂AB一8分离纯化桅子总普和桅子黄色素的工艺条件;同时还研究了9种大孔吸附树脂对贯叶金丝桃中黄酮类化合物的吸附性能，其中比吸附量较大的树脂型号是:HPDSOO、HPDIOO、AB一8和NKA一9。 此外，总结了大孔吸附树脂的性能、种类、吸附原理及在医药工业中的研究应用情况，重点对大孔吸附树脂在中药和天然产物有效成分分离纯化中的研究进展作了比较一详细的综述。更多还原

【Abstract】 Macroporous adsorption resin(MAR) is an adsorptive polymer with macroreticular structure. In recent years, MAR has been used in the seperation and purification of TCM and natural products more broadly for its special adsorption performance to water soluble materials. Now, Some organic residues still remain in most of the commercial MARs produced by domestic factories, which induces the unsafely of the drugs performed by MARs. In order to build a simple analytical method of the residues of MARs and effective elution method of MARs, we performed the following experiments.Organic residues in nine kinds MARs were identified by GC-MS. Toluene, diethylbenzene and naphthalene existed in all MARs. The other benzene derivatives, such as xylene, strylene, divinylbenzene and other residues were also identified, but their quantities were little. Dozens of alkanes were also detected. Among them, the quantities of decane, undecane and dodecane were very high.During studied the pretreatment method of MAR detected by GC and UV, we found that solvent and tempreture were two key elements in this procedure. Under a certain tempreture, MAR was almost clean after it was eluted by 5% NaOH for 2 bed volume of MAR(BV) and then by organic solvent for only 3~5BV. The operation is easy, short time and had little contamination to the environment. The amount of solvent used in the pretreatment were little. Besides, We found that when the absorbance value was 0.2~0.4( λ =254nm), the organic residues were also very limited detected by GC. That was the absorbance value could represent the amount of the organic residues in some extent and we could use the UV method to detect the organic residues of MARs conveniently.A method was established to detect the organic residues in MARs and medicines with GC method. The detection was easy and sensitive. All the ten organic residues could be determined through a column simultaneously in a short time.A standard was also made for medicinal MARs: in the dried MARs, benzene shouldn’t be more than 2ppm; toluene, xylene, strylene, diethylbenzene, divinylbenzene, naphthalene, decane, undecane and dodecane should’t be more than 20ppm.We also studied the application of MARs in the seperation and purification of TCM. The main active components of Gardenia jasminoides Ellis, and Hypericum perforatum L.were gardenoside, crocins and flavonoids. But studies on the seperation and purification of active components in both plants by MARs had not been reported. We studied the adsorption performance of 13 MARs to irodoids in Gardenia jasminoides Ellis. Among them, HPD-100,AB-8, SP825 and SP207 had a bigger adsorption capacities. Resin AB-8 had a good seperation performance. At the same time, we established a method of seperation and purification of the yellow pigment and the total glycosides in Gardenia jasminoides Ellis by resin AB-8. We also studied adsortion performance of 9 resins to flavonoids in Hypericum perforatum L. Among them, resin HPD-500, HPD100, AB-8 and NKA-9 had a bigger adsorption capacities.Advance in the types, properties, principle of adsorption of MARs and their application in the medical and pharmerceutical industry were summerized, especially the research and development of MARs on the seperation and purification of the active components in TCM and natural products were emphasized.更多还原