CN106421338A - 一种增液颗粒及其制备方法 - Google Patents
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Abstract
本发明提供一种增液颗粒及其提取方法,取玄参270g、地黄216g、麦冬216g,加药材10倍重量的水,浸泡0.5h,煎煮1小时,过滤,药渣再加入药材8倍重量的水,煎煮1小时,药液滤出等步骤,并采用特有的颗粒干燥设备,制备得到的增液颗粒中哈巴俄苷含量高,并且发现增液颗粒在制备抑制中国仓鼠卵巢CHO细胞增殖药物中的应用。
Description
技术领域
本发明涉及中药提取技术领域,具体涉及一种增液颗粒及其制备方法。
背景技术
增液颗粒养阴生津,清热润燥。用于热邪伤阴、津液不足所引起的阴虚内热,口干咽燥,大便燥结;亦可用于感染性疾患高热所致体液耗损的辅助用药。现有技术中的制备方法,工艺粗糙、落后,杂质多,有效成分含量低,导致患者用量过大,不方便服用,严重影响了本品在临床上应用。
发明内容
发明目的:为了解决上述问题,本发明的目的在于提供一种增液颗粒及其制备方法。
技术方案:本发明的目的是通过如下的方案实现的:
一种增液颗粒,制备方法为:取玄参270g、地黄216g、麦冬216g,加药材10倍重量的水,浸泡0.5h,煎煮1小时,过滤,药渣再加入药材8倍重量的水,煎煮1小时,药液滤出,合并两次煎煮液,减压浓缩至60℃相对密度为1.05,加乙醇使含醇量的体积百分比达75%,搅拌,静置,过滤,滤液减压浓缩至65℃时相对密度为1.25,并回收乙醇,得浓缩液,使用硅胶精制,预先将选定的硅胶装入树脂柱中,同时将所述浓缩液经纯化水稀释后,通过反相硅胶柱,去掉液体中的杂质,收集全部流出液,继续减压浓缩,将浓缩液进行喷雾干燥,制粒,颗粒干燥,得增液颗粒。
所述一种增液颗粒,制备方法中所述硅胶比表面为300~500m2/g,孔容为0.70~0.90ml/g,所述稀释后浓缩液通过反相硅胶柱分离、洗脱,至出水无色止。
所述增液颗粒,上述制备方法中颗粒干燥使用装置,包括:机壳、滚筒以及进料斗,其特征在于:所述机壳为圆筒状,固定安装在支架上,机壳底部设置出料口,其内安装滚筒,所述滚筒上设固定若干个畚斗,畚斗由两块对称的弧形板拼接而成,畚斗的顶端靠近机壳的内壁,滚筒为中空圆柱形筒体,其内表面安装一层电加热板,所述电加热板连接电源电路,滚筒的一端固定带轮,所述带轮通过皮带连接电机;机壳的左上方设置进料口,所述进料口与进料斗连接;机壳的顶部设置开口,所述开口连接管道,所述管道的一端安装抽气扇。
所述增液颗粒的制备方法,上述提取方法中所述滚筒的表面沿滚筒的轴向均匀设置若干条形凹槽。
所述增液颗粒的制备方法,上述提取方法中所述机壳上设置控制面板,所述控制面板包括一个调速按钮,所述调速按钮与电机的控制电路连接。
所述增液颗粒在制备抑制中国仓鼠卵巢CHO细胞增殖药物中的应用。
现有技术中,增液颗粒采用水提的方法,工艺粗糙、落后,杂质多,导致患者用量过大,不方便服用,本发明制备的增液颗粒哈巴俄苷得率增加,含量高。本发明中的颗粒干燥设备结构简单、操作简单快捷,能有效实现药物颗粒的除湿干燥,且造价较低,适合广泛推广,并且发现增液颗粒在制备抑制中国仓鼠卵巢CHO细胞增殖药物中的应用。
附图说明
为了使本发明的内容更容易被清楚的理解,下面根据具体实施例并结合附图,对本发明作进一步详细的说明,其中:
图1为本发明颗粒干燥装置的结构示意图。
图2为本发明颗粒干燥装置中滚筒的结构示意图。
具体实施方式
以下通过实施例形式,对本发明的上述内容再作进一步的详细说明,但不应将此理解为本发明上述主题的范围仅限于以下的实例,凡基于本发明上述内容所实现的技术均属于本发明的范围。
实施例1
取玄参270g、地黄216g、麦冬216g,加药材10倍重量的水,浸泡0.5h,煎煮1小时,过滤,药渣再加入药材8倍重量的水,煎煮1小时,药液滤出,合并两次煎煮液,减压浓缩至60℃相对密度为1.05,加乙醇使含醇量的体积百分比达75%,搅拌,静置,过滤,滤液减压浓缩至65℃时相对密度为1.25,并回收乙醇,得浓缩液,使用硅胶精制,预先将选定的硅胶装入树脂柱中,同时将所述浓缩液经纯化水稀释后,通过反相硅胶柱,去掉液体中的杂质,收集全部流出液,继续减压浓缩,将浓缩液进行喷雾干燥,制粒,颗粒干燥,得增液颗粒,每袋10g。
所述增液颗粒的制备方法,所述硅胶精制方法为:预先将选定的硅胶装入树脂柱中,同时将所述浓缩液经纯化水稀释后,通过反相硅胶柱,去掉液体中的杂质,收集全部流出液。
所述增液颗粒的制备方法,所述硅胶比表面为300m2/g,孔容为0.90ml/g,所述稀释后浓缩液通过反相硅胶柱分离、洗脱,至出水无色止。
所述增液颗粒的制备方法,上述颗粒干燥使用装置,见图1-2,包括:机壳3、滚筒5以及进料斗7,所述机壳3为圆筒状,固定安装在支架2上,机壳3底部设置出料口1,其内安装滚筒5,所述滚筒5上设固定若干个畚斗4,畚斗4由两块对称的弧形板拼接而成,畚斗4的顶端靠近机壳3的内壁,滚筒5为中空圆柱形筒体,其内表面安装一层电加热板12,所述电加热板12连接电源电路,用于将滚筒5的表面加热,滚筒5的一端固定带轮11,所述带轮11通过皮带连接电机;机壳3的左上方设置进料口6,所述进料口6与进料斗7连接,颗粒从进料口6进入机壳3内,并由畚斗4运转,随着滚筒5转动,在转动过程中,颗粒与畚斗4和滚筒5外表面接触,利用畚斗4与滚筒5表面的热量将颗粒中的水蒸气蒸发出来,达到除湿的目的,最终由出料口1被收集起来;机壳3的顶部设置开口,所述开口连接管道9,所述管道9的一端安装抽气扇8,用于将干燥过程中蒸发出来的水蒸气抽出机壳3外。
所述滚筒5的表面沿滚筒5的轴向均匀设置若干条形凹槽13,条形凹槽13增大了颗粒与滚筒5表面的摩擦,使颗粒不易轻易滑动,其加热的时间也就更长,且条形凹槽13增加了滚筒5表面有效加热面积,使干燥更充分彻底。
所述机壳3上设置控制面板,所述控制面板包括一个调速按钮10,所述调速按钮10与电机的控制电路连接,可实现控制电机转速,即控制滚筒5转速,不同批次的颗粒的含水量可能是不一样的,针对需要不同干燥程度的颗粒调节不同的滚筒5转速,改变颗粒在滚筒5上停留的时间,从而实现不同的干燥效果。
实施例2
取玄参270g、地黄216g、麦冬216g,加药材10倍重量的水,浸泡0.5h,煎煮1小时,过滤,药渣再加入药材8倍重量的水,煎煮1小时,药液滤出,合并两次煎煮液,减压浓缩至60℃相对密度为1.05,加乙醇使含醇量的体积百分比达75%,搅拌,静置,过滤,滤液减压浓缩至65℃时相对密度为1.25,并回收乙醇,得浓缩液,使用硅胶精制,预先将选定的硅胶装入树脂柱中,同时将所述浓缩液经纯化水稀释后,通过反相硅胶柱,去掉液体中的杂质,收集全部流出液,继续减压浓缩,将浓缩液进行喷雾干燥,制粒,颗粒干燥,得增液颗粒,每袋10g。
所述增液颗粒的制备方法,所述硅胶精制方法为:预先将选定的硅胶装入树脂柱中,同时将所述浓缩液经纯化水稀释后,通过反相硅胶柱,去掉液体中的杂质,收集全部流出液。
所述一种增液颗粒的制备方法,所述硅胶比表面为500m2/g,孔容为0.70ml/g,所述稀释后浓缩液通过反相硅胶柱分离、洗脱,至出水无色止。
颗粒干燥设备同上。
实施例3
取玄参270g、地黄216g、麦冬216g,加药材10倍重量的水,浸泡0.5h,煎煮1小时,过滤,药渣再加入药材8倍重量的水,煎煮1小时,药液滤出,合并两次煎煮液,减压浓缩至60℃相对密度为1.05,加乙醇使含醇量的体积百分比达75%,搅拌,静置,过滤,滤液减压浓缩至65℃时相对密度为1.25,并回收乙醇,得浓缩液,使用硅胶精制,预先将选定的硅胶装入树脂柱中,同时将所述浓缩液经纯化水稀释后,通过反相硅胶柱,去掉液体中的杂质,收集全部流出液,继续减压浓缩,将浓缩液进行喷雾干燥,制粒,颗粒干燥,得增液颗粒,每袋10g。
所述增液颗粒的制备方法,所述硅胶精制方法为:预先将选定的硅胶装入树脂柱中,同时将所述浓缩液经纯化水稀释后,通过反相硅胶柱,去掉液体中的杂质,收集全部流出液。
所述一种增液颗粒的制备方法,所述硅胶比表面为400m2/g,孔容为0.80ml/g,所述稀释后浓缩液通过反相硅胶柱分离、洗脱,至出水无色止。
颗粒干燥设备同上。
上述实施例中药材符合药典标准。
实施例4:本发明增液颗粒中哈巴俄苷含量测定实验研究资料
1.1实验药物:本发明增液颗粒:按实施例1-3方法制备。对照组采用普通颗粒干燥方法制备增液颗粒。
1.2仪器:高效液相色谱仪系统包括高效液相色谱仪(Waters 515);P200高压泵;Waters 2487紫外检测器及GJ605型高压六通进样阀;色谱柱为BDS HYPERSIL-C18(4.6mm×250mm,5μm);数据采集及处理采用HS色谱数据工作站V4.0+(杭州英谱科技)
1.3测定条件:照高效液相色谱法(通则0512)测定。色谱条件与系统适用性试验以十八烷基硅烷键合硅胶为填充剂;以乙腈-1%冰醋酸溶液(27∶73),为流动相;检测波长为278nm;理论板数按哈巴俄苷峰计算应不低于2000。取哈巴俄苷对照品适量,精密称定,加甲醇制成每lm l含5ug的溶液,即得。供试品溶液的制备取装量差异项下的本品,研细,取约0.5g,精密称定,置25ml量瓶中,加甲醇20ml,超声处理(功率250W,频率40kHz)30分钟,放冷,加甲醇至刻度,摇匀,滤过,取续滤液,即得。分别精密吸取对照品溶液与供试品溶液各20ul注入液相色谱仪,测定,即得。
1.4实验结果
各实施例制备的增液颗粒中哈巴俄苷含量测定结果
样品来源 | 哈巴俄苷含量(mg/袋) |
实施例1 | 1.2 |
实施例2 | 1.5 |
实施例3 | 2.1 |
对照组 | 0.4 |
根据上表的试验结果可知,本发明实施例1-3制备的增液颗粒中哈巴俄苷含量明显高于对照组。
实施例5:本发明增液颗粒抑制中国仓鼠卵巢CHO细胞增殖的实验研究资料
1实验材料
1.1实验用细胞株
中国仓鼠卵巢CHO细胞,南京医科大学实验室细胞库,DMEM+10%FBS常规培养。
1.2实验药物
研究药物:本发明增液颗粒:按实施例1方法制备。
药液储液:称取100mg增液颗粒,溶于5ml无水乙醇中,0.2μm滤器过滤,500μl doff管分装,-20℃存储,同时0.2μm滤器过滤无水乙醇以备对照组之用。
1.3实验试剂
DMEM(GIBCO公司Cat.No.12100-061Lot.No.758137);胎牛血清(浙江天杭生物科技有限公司Lot.No.100419);NaHCO3(上海久亿化学试剂有限公司Cat. No.11810-033Lot.No.1088387);Trypsin(AMRESCO公司批号:2010/04);EDTA(AMRESCO公司批号:2009/10);Penicillin G Sodium Salt(AMRESCO公司批号:2010242);StreptomycinSulfate(AMRESCO公司批号:2010382);无水乙醇(南京化学试剂有限公司批号:080310182);MTT(Biosharp批号:0793);PBS(实验室自配);
1.4实验器材
莱卡倒置显微镜(德国Leica型号:DM1L);可见-紫外光微孔板检测仪(美国MD公司型号:SPECTRA MAX 190);CO2培养箱(FORMA型号:3111);超净台(苏净集团安泰公司制造型号:SW-CJ-ZFD);纯水仪(美国Spring公司型号:S/N 020579);精密移液器(法国吉尔森公司型号:P2);电子天平(德国赛多利斯有限公司型号:BT323S);全自动高压灭菌锅(日本SANYO公司型号:MLS-3020);台式电热鼓风干燥箱(上海精密实验设备公司型号:DHG9123A);冰箱(西门子公司型号:KG18V21TI);液氮罐(CBS型号:2001);低速离心机(上海安亭科学仪器厂型号:KA-1000);0.2μm滤器(MILLIPORE型号:SLGP033RB);10cm培养皿(NEST公司)、96孔培养板(NEST公司);细胞计数板;离心管、移液管、Tips若干。
2实验方法
1)中国仓鼠卵巢CHO细胞用DMEM+10%FBS于37℃、5%CO2进行常规培养(10cm培养皿),当细胞生长至对数期时,收集细胞,弃去培养液,PBS轻洗3遍,加入3ml 0.25%胰蛋白酶-0.04%EDTA,37℃消化2min后,向其中加入5ml完全培养基中和反应,吹打细胞后将其转入离心管中,1000rpm离心5min,调整细胞悬液浓度3×104个/ml。
2)将细胞种入96孔培养板中,每孔加入细胞悬液180μl,培养板放入细胞培养箱中(37℃,5%CO2)常规培养。
3)根据细胞生长情况,一般长至50%-70%,加入增液颗粒溶液,继续培养24h。
4)24h后加入20μl MTT溶液(5mg/ml,即0.5%MTT),继续培养4h。
5)4h后扣板法倒去上清,用吸水纸轻轻拍干,每孔加入200μl二甲基亚砜,置摇床上低速振荡10min,使结晶物充分溶解。在酶联免疫检测仪490nm处测量各孔的吸光值。
6)同时设置本底(不加细胞,只加培养液),对照孔(细胞、相同浓度的药物溶解介质、培养液、MTT、二甲基亚砜),每组设定6个复孔。
7)结果以药物对细胞的抑制率表示:
细胞增值抑制率(%)=(对照孔OD值-给药孔OD值)/对照孔OD值×100%。实验重复3次。
3统计处理
采用Microsoft Excel 2003软件中的相关分析和Student t检验,数据以mean±S.D.表示。
4实验结果
MTT法实验后统计结果显示,与对照组比较,当剂量达到5mg/ml时,对中国仓鼠卵巢CHO细胞增殖抑制有差异(P<0.05),剂量在10mg/ml时该差异具有显著性(P<0.01),当剂量达到15-20mg/ml时有极显著性差异(P<0.001)。
增液颗粒对中国仓鼠卵巢CHO细胞增殖抑制影响研究
注:与对照组比较,*P<0.01;**P<0.001
5实验结论
增液颗粒可以抑制中国仓鼠卵巢CHO细胞增殖,减少中国仓鼠卵巢CHO细胞的细胞生长数目,该作用呈剂量依赖性。
Claims (6)
1.一种增液颗粒,其特征在于制备方法为:取玄参270g、地黄216g、麦冬216g,加药材10倍重量的水,浸泡0.5h,煎煮1小时,过滤,药渣再加入药材8倍重量的水,煎煮1小时,药液滤出,合并两次煎煮液,减压浓缩至60℃相对密度为1.05,加乙醇使含醇量的体积百分比达75%,搅拌,静置,过滤,滤液减压浓缩至65℃时相对密度为1.25,并回收乙醇,得浓缩液,使用硅胶精制,预先将选定的硅胶装入树脂柱中,同时将所述浓缩液经纯化水稀释后,通过反相硅胶柱,去掉液体中的杂质,收集全部流出液,继续减压浓缩,将浓缩液进行喷雾干燥,制粒,颗粒干燥,得增液颗粒。
2.根据权利要求1所述增液颗粒,其特征在于制备方法中所述硅胶比表面为300~500m2/g,孔容为0.70~0.90ml/g,所述稀释后浓缩液通过反相硅胶柱分离、洗脱,至出水无色止。
3.根据权利要求1所述增液颗粒,其特征在于上述提取方法中颗粒干燥使用装置,包括:机壳、滚筒以及进料斗,其特征在于:所述机壳为圆筒状,固定安装在支架上,机壳底部设置出料口,其内安装滚筒,所述滚筒上设固定若干个畚斗,畚斗由两块对称的弧形板拼接而成,畚斗的顶端靠近机壳的内壁,滚筒为中空圆柱形筒体,其内表面安装一层电加热板,所述电加热板连接电源电路,滚筒的一端固定带轮,所述带轮通过皮带连接电机;机壳的左上方设置进料口,所述进料口与进料斗连接;机壳的顶部设置开口,所述开口连接管道,所述管道的一端安装抽气扇。
4.根据权利要求3所述增液颗粒的制备方法,其特征在于上述提取方法中所述滚筒的表面沿滚筒的轴向均匀设置若干条形凹槽。
5.根据权利要求3所述增液颗粒的制备方法,其特征在于上述提取方法中所述机壳上设置控制面板,所述控制面板包括一个调速按钮,所述调速按钮与电机的控制电路连接。
6.根据权利要求1所述增液颗粒在制备抑制中国仓鼠卵巢CHO细胞增殖药物中的应用。
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