CN111198240B - 一种茶叶中提取1，2，6三没食子酰葡萄糖的方法 - Google Patents
一种茶叶中提取1，2，6三没食子酰葡萄糖的方法 Download PDFInfo
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- 241001122767 Theaceae Species 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 18
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000000605 extraction Methods 0.000 claims abstract description 7
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 8
- 239000012043 crude product Substances 0.000 claims description 6
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 4
- 239000000284 extract Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 2
- 229930014626 natural product Natural products 0.000 abstract description 2
- 235000013616 tea Nutrition 0.000 description 27
- 229920002203 1,2,6-Trigalloyl glucose Polymers 0.000 description 5
- 239000000706 filtrate Substances 0.000 description 4
- 238000004128 high performance liquid chromatography Methods 0.000 description 4
- 239000003814 drug Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- QJYNZEYHSMRWBK-NIKIMHBISA-N 1,2,3,4,6-pentakis-O-galloyl-beta-D-glucose Chemical compound OC1=C(O)C(O)=CC(C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(O)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(O)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(O)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(O)C(O)=C(O)C=2)=C1 QJYNZEYHSMRWBK-NIKIMHBISA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 244000052616 bacterial pathogen Species 0.000 description 2
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- 230000008025 crystallization Effects 0.000 description 2
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- 238000001035 drying Methods 0.000 description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 2
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Abstract
一种茶叶中提取1，2，6三没食子酰葡萄糖的方法，属于属于天然物提取技术领域。该方法为：取茶叶采用乙醇或甲醇溶液提取得到1，2，6三没食子酰葡萄糖。上述一种茶叶中提取1，2，6三没食子酰葡萄糖的方法，具有简单、高效的特点，可大大提高茶叶中提取1，2，6三没食子酰葡萄糖的含量，同时也是提高茶叶附加值的理想方法。
Description
技术领域
本发明属于天然物提取技术领域，具体涉及一种茶叶中提取1，2，6三没食子酰葡萄糖的方法。
背景技术
天然1，2，6三没食子酰葡萄糖在消炎、抑制耐药性病原菌等方面具有明显作用，已有研究发现其消炎效果优于已广泛使用的五没食子酰葡萄糖，配合抗生素使用后对泌尿系耐药病原菌的抗性可从小于30%提高到90%以上。但由于天然1，2，6三没食子酰葡萄糖在一般植物中含量较低，目前市场上没有相应的纯合物，限制了它在商业上的开发利用。
近年来我们首次从茶叶中分离到特异成分1，2，6三没食子酰葡萄糖的纯合物，在一些特异品种资源中其含量较高，因此如何从茶叶中提取高纯度1，2，6三没食子酰葡萄糖是促进该物质在医学、商业等领域应用的关键。
发明内容
针对现有技术存在的问题，本发明的目的在于设计提供一种茶叶中提取1，2，6三没食子酰葡萄糖的方法的技术方案。
所述的一种茶叶中提取1，2，6三没食子酰葡萄糖的方法，其特征在于取茶叶采用乙醇或甲醇溶液提取得到1，2，6三没食子酰葡萄糖。
所述的一种提取1，2，6三没食子酰葡萄糖的方法，其特征在于所述乙醇或甲醇提取液浓度为50-100%，提取方式为浸泡提取。
所述的一种提取1，2，6三没食子酰葡萄糖的方法，其特征在于取乙醇或甲醇溶液提取得到的1，2，6三没食子酰葡萄糖提取液，浓缩，上C18反相柱反复过柱，以甲醇-水梯度洗脱，得到1，2，6三没食子酰葡萄糖粗品。
所述的一种提取1，2，6三没食子酰葡萄糖的方法，其特征在于取1，2，6三没食子酰葡萄糖粗品上高压制备仪时，以乙腈：磷酸水为20:80为流动相，得到1，2，6三没食子酰葡萄糖次精品。
所述的一种提取1，2，6三没食子酰葡萄糖的方法，其特征在于取1，2，6三没食子酰葡萄糖精品低温结晶，得到1，2，6三没食子酰葡萄糖精品。
上述一种茶叶中提取1，2，6三没食子酰葡萄糖的方法，具有简单、高效的特点，可大大提高茶叶中提取1，2，6三没食子酰葡萄糖的含量，同时也是提高茶叶附加值的理想方法。
具体实施方式
以下结合实施例来进一步说明本发明。
实施例1
1）茶样制备：在春茶季节采摘缙云黄茶头茶样品（一芽一叶），制成干茶后用磨样机磨成茶粉。
2）样品提取：称取茶样230 g，加20倍量的70%乙醇水浸泡1天。用滤布滤出滤液，残渣再加20倍量的70%乙醇水浸泡1天。滤出滤液。合并两次的提取液，用硅藻土再次过滤。得到的上清液,旋转蒸发仪浓缩后，上C18反相柱，以甲醇-水按10%甲醇-40%甲醇梯度洗脱。用高效液相（大连依利特高效液相仪）检测各馏分。
3）将含有1，2，6三没食子酰葡萄糖的馏分合并，浓缩，再次上C18反相柱。经反复过柱4-5次，得60%纯度的1，2，6三没食子酰葡萄糖粗品610mg。
4）将60%纯度的1，2，6三没食子酰葡萄糖粗品上高压制备仪（苏州汇通高压制备仪HT7050A），用乙腈：磷酸水=20:80为流动相，制备得到90%纯度的1，2，6三没食子酰葡萄糖次精品260mg。
5）将1，2，6三没食子酰葡萄糖次精品浓缩至20mL，放4℃冰箱中析晶。结晶析出后，滤出，干燥，得纯度98%以上的1，2，6三没食子酰葡萄糖精品150mg。
实施例2
1）茶样制备：在春茶季节采摘缙云黄茶头茶样品（一芽一叶），制成干茶。
2）样品提取：称取茶样200 g，加20倍量的70%甲醇水浸泡1天。用滤布滤出滤液，残渣再加20倍量的70%甲醇水浸泡1天。滤出滤液。合并两次的提取液，用硅藻土再次过滤。得到的上清液,旋转蒸发仪浓缩后，上C18反相柱，以甲醇-水按10%甲醇-40%甲醇梯度洗脱。用高效液相（大连依利特高效液相仪）检测各馏分。
3）将含有1，2，6三没食子酰葡萄糖的馏分合并，浓缩，再次上C18反相柱。经反复过柱4-5次，得62%纯度的1，2，6三没食子酰葡萄糖粗品1.7g。
4）将62%纯度的1，2，6三没食子酰葡萄糖粗品上高压制备仪（苏州汇通高压制备仪HT7050A），用乙腈：磷酸水=20:80为流动相，制备得到91%纯度的1，2，6三没食子酰葡萄糖次精品920mg。
5）将1，2，6三没食子酰葡萄糖次精品浓缩至约20mL，放4℃冰箱中析晶。结晶析出后，滤出，干燥，得纯度98%以上的1，2，6三没食子酰葡萄糖精品555mg。
结果发现采用茶叶直接提取，同时提取液选择70%甲醇效果优于茶叶磨成茶粉及提取液选择乙醇效果。
Claims (3)
1.一种茶叶中提取1，2，6三没食子酰葡萄糖的方法，其特征在于取茶叶采用乙醇溶液或甲醇溶液提取得到1，2，6三没食子酰葡萄糖；取乙醇溶液或甲醇溶液提取得到的1，2，6三没食子酰葡萄糖提取液，浓缩，上C18反相柱反复过柱，以甲醇-水梯度洗脱，得到1，2，6三没食子酰葡萄糖粗品；取1，2，6三没食子酰葡萄糖粗品上高压制备仪时，以乙腈：磷酸水为20:80为流动相，得到1，2，6三没食子酰葡萄糖次精品。
2.如权利要求1所述的一种茶叶中 提取1，2，6三没食子酰葡萄糖的方法，其特征在于所述乙醇溶液的浓度为50-100%，甲醇溶液的浓度为50-100%，提取方式为浸泡提取。
3.如权利要求1所述的一种茶叶中 提取1，2，6三没食子酰葡萄糖的方法，其特征在于取1，2，6三没食子酰葡萄糖次 精品低温结晶，得到1，2，6三没食子酰葡萄糖精品。
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