CN110755552B - 一种叠鞘石斛粉的制备方法 - Google Patents
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Abstract
本发明涉及一种叠鞘石斛粉的制备方法;包括以下步骤:(1)清洗处理:将新鲜叠鞘石斛去除叶片,放入清洗液中浸泡清洗,捞出脱除其表面的水分,备用:(2)烘干:将脱水后的叠鞘石斛烘干至含水量为60‑70%后,切片;(3)冷冻处理:将石斛片冷冻;(4)压差膨化处理:将冷冻石斛片进行压差膨化,制得膨化石斛片;(5)低温回流提取浓缩:将膨化石斛片加入有机溶剂进行低温回流提取浓缩,制得一次浓缩物;(6)浓缩:将一次浓缩物送到球形真空浓缩罐中浓缩,制得二次浓缩物;(7)干燥粉碎:将二次浓缩液干燥后,再粉碎,制得粗叠鞘石斛粉;(8)配料。本发明提供的方法,叠鞘石斛生物活性成分损失率小,溶解浸出率高,生物吸收利用度高。
Description
技术领域
本发明属于药材提取技术领域,尤其涉及一种叠鞘石斛粉的制备方法。
背景技术
叠鞘石斛是是兰科石斛属植物线叶石斛的一个变种,主要分布在我国四川省西南部、广西西南至西北部、贵州南部、云南东南部等地。目前在四川省乐山市夹江县广为栽培并供药用。叠鞘石斛与原变种的区别在于植株明显较粗壮,茎粗4毫米以上,叶宽1.8~4.5厘米,花序长5~14厘米,花苞片长1.8~3厘米,唇瓣上面具一个大的紫色斑块。叠鞘石斛中主要含有多糖类、鞣质、联苄类、生物碱、香豆素类、糖类、苷类、菲类、芴酮类和三萜类化合;具有益胃生津,滋阴清热的作用,临床上被广泛用于治疗慢性萎缩性胃炎、抗肿瘤、抗衰老、增强机体免疫力等疾病。
由于叠鞘石斛具有良好的药用价值和保健价值,人们对其需求量日益增多,前人们喜欢直接食用石斛鲜条,或者将石斛鲜条榨汁后直接饮用,但从市面直接购得的石斛鲜条保存时间相对较短,易发生腐烂霉变。传统上,人们将铁皮石斛干燥加工成“枫斗”来延长其保存时间,因其属于热干产品,产品不可避免地出现收缩、硬化、色变和难以复水等现象,且食用是需至少要几个小时的温煮或包烫,极其不方便,其有效成分的无法充分溶出与吸收。因此,不少研究者将石斛通过一定工艺加工成石斛粉末,来提高其有效成分的吸收溶出。如公开号为CN106389874A的中国专利公开了一种可直接口服中药饮片铁皮石斛粉的制备方法,包括如下步骤:(1)灭菌:将铁皮石斛置于臭氧水内进行臭氧灭菌;(2)粉碎:利用湿法粉碎对铁皮石斛进行粉碎处理,得到铁皮石斛浆液;(3)过滤:利用滤网将铁皮石斛浆液进行真空抽滤,得到滤浆;(4)浓缩:将所述滤浆进行真空减压浓缩,得到浓浆;(5)干燥:将所述浓浆进行真空冷冻干燥,得到铁皮石斛粉。又如公开号为CN110368454A的专利公开了一种石斛粉末中药饮片及其制备方法,包括如下步骤:将石斛鲜茎条洗净沥干后,进行晾晒,得到经过预处理的石斛;将石斛置于臭氧水内进行臭氧灭菌;将石斛清洗后,加入纯化水进行湿法粉碎,得到石斛浆液;将石斛浆液中加入复合酶解剂进行酶解,得到酶解浆液,然后进行超声波破壁处理;对经过超声波破壁处理的酶解浆液进行真空抽滤,得到石斛滤浆;对石斛滤浆进行真空减压浓缩,得到石斛浓浆;将石斛浓浆真空冷冻干燥;得到石斛粉末中药饮片。
上述专利提供的方法降低了石斛中有效成分的损失率,但石斛粉中活性成分溶解度小,生物吸收利用度还是较低。
发明内容
为了解决现有技术中存在的上述技术问题,本发明提供了一种叠鞘石斛粉的制备方法,具体是通过以下技术方案实现的:
一种叠鞘石斛粉的制备方法,包括以下步骤:
(1)清洗处理:将新鲜叠鞘石斛去除叶片,放入清洗液中浸泡清洗6-8min,然后捞出送到脱水机中脱除其表面的水分,备用:
(2)烘干:将脱水后的叠鞘石斛送到热风循环烘箱中,在50-60℃下烘干至含水量为60-70%后,切成石斛片;
(3)冷冻处理:将石斛片在-15℃~-18℃下冷冻15-20h;
(4)压差膨化处理:将冷冻石斛片添加到膨化罐内进行压差膨化,制得膨化石斛片;
(5)低温回流提取浓缩:将膨化石斛片添加到热回流低温提取低温浓缩机中,加入其质量8-10倍有机溶剂进行低温回流提取浓缩,制得一次浓缩物;
(6)浓缩:将一次浓缩物送到球形真空浓缩罐中浓缩,制得二次浓缩物;
(7)干燥粉碎:将二次浓缩物送到高真空干燥机干燥后,再经无尘粉碎机粉碎至200-300目,制得粗叠鞘石斛粉;
(8)配料:将粗叠鞘石斛粉与其质量1-2%的辅料搅拌混合均匀,即得叠鞘石斛粉。
优选地,所述清洗液中含有1-2%肉桂酸、0.5-1%甘草素、1-2%抗坏血酸、4-5%大蒜素、3-4%植酸、0.1-0.2%渗透压调节剂,其余为水。
优选地,所述渗透压调节剂为氯化钙。
优选地,所述压差膨化为:将膨化罐内的压力保持在0.05Pa,加热至60℃,保持该温度和压力20s,之后控制压力瞬间降低至-0.08MPa,即得膨化石斛片。
优选地,所述步骤(5)的膨化石斛片低温回流提取前经经过了发酵处理,发酵处理的方法为:向膨化石斛片中加入其质量0.1-0.15%的石斛花精油,然后加入其质量0.01-0.02%的菌液在25-30℃发酵8-10h,灭菌后再进行低温回流提取。
优选地,所述菌液为解淀粉芽孢杆菌菌液,其活菌数为1-2×106cfu/ml。
优选地,所述步骤(5),有机溶剂为80%乙醇,低温回流提取浓缩的条件为:提取罐内压力0.03MPa,罐内温度55-80℃,浓缩比重1.2-1.35。
优选地,所述步骤(8),辅料为微晶纤维素。
本发明的有益效果在于:
本发明采用清洗液对叠鞘石斛进行浸泡清洗,清洗液中含有肉桂酸、甘草素、抗坏血酸等物质,对叠鞘石斛内的氧化酶具有较强的抑制作用,同时具有良好的抑菌效果;在渗透压调节剂的作用下能渗透到叠鞘石斛细胞中,能有效防止叠鞘石斛发生氧化而导致其营养成分损失。将石斛片经冷冻处理后进行膨化处理,石斛片中的水分在冷冻条件下变成结晶水,压差膨化处理这部分结晶水会迅速升华而使石斛粉膨化,从而达到破坏石斛片植物细胞的效果,提高其中有效成分的溶出。采用解淀粉芽孢杆菌菌液对添加了石斛花精油的膨化石斛粉进行发酵处理,在石斛花精油的诱导下,解淀粉芽孢杆菌能发酵产生生物表面活性剂,进而能提高石斛粉与机体的生物相容性,提高其生物利用度;同时还能提高石斛粉中有效成分的溶解度。采用中药热回流低温提取低温浓缩机对石斛片进行提取浓缩,提取时处于真空负压能加快细胞膨胀,细胞膜结构破坏,细胞有成分不断溶出;且回流的溶剂反复运动于药材表面,能提高溶剂对药材的摩擦洗脱力与溶解度;能有效提高药材的提取率与石膏率。采用微晶纤维素对叠鞘石斛粉进行配料能进一步增加石斛粉的溶解率,提高起生物利用度。
本发明提供的叠鞘石斛粉的制备方法,生物活性成分损失率小,溶解浸出率高,生物吸收利用度高。
具体实施方式
下面结合具体的实施方式来对本发明的技术方案做进一步的限定,但要求保护的范围不仅局限于所作的描述。
实施例1
一种叠鞘石斛粉的制备方法,包括以下步骤:
(1)清洗处理:将新鲜叠鞘石斛去除叶片,放入清洗液中浸泡清洗6min,然后捞出送到脱水机中脱除其表面的水分,备用:
(2)烘干:将脱水后的叠鞘石斛送到热风循环烘箱中,在50-60℃下烘干至含水量为60-70%后,切成石斛片;
(3)冷冻处理:将石斛片在-15℃下冷冻20h;
(4)压差膨化处理:将冷冻石斛片添加到膨化罐内进行压差膨化,制得膨化石斛片;
(5)低温回流提取浓缩:将膨化石斛片添加到热回流低温提取低温浓缩机中,加入其质量8倍的有机溶剂低温回流提取浓缩8h,制得一次浓缩物;
(6)浓缩:将一次浓缩物送到球形真空浓缩罐中浓缩,制得二次浓缩物;
(7)干燥粉碎:将二次浓缩物送到高真空干燥机干燥后,再经无尘粉碎机粉碎至200-300目,制得粗叠鞘石斛粉;
(8)配料:将粗叠鞘石斛粉与其质量1-2%的微晶纤维素搅拌混合均匀,即得叠鞘石斛粉。
所述清洗液中含有1%肉桂酸、0.5%甘草素、1%抗坏血酸、4%大蒜素、3%植酸、0.1%氯化钙,其余为水。
所述压差膨化为:将膨化罐内的压力保持在0.05Pa,加热至60℃,保持该温度和压力20s,之后控制压力瞬间降低至-0.08MPa,即得膨化石斛片。
所述步骤(5)的膨化石斛片低温回流提取前还经过了发酵处理,发酵处理的方法为:向膨化石斛片中加入其质量0.1%的石斛花精油,然后加入其质量0.01%的菌液在25-30℃发酵8h,灭菌后再进行低温回流提取。
所述菌液为解淀粉芽孢杆菌菌液,其活菌数为1-2×106cfu/ml。
所述步骤(5),有机溶剂为80%乙醇,低温回流提取浓缩的条件为:提取罐内压力0.03MPa,罐内温度55-80℃,浓缩比重1.2-1.35。
实施例2
一种叠鞘石斛粉的制备方法,包括以下步骤:
(1)清洗处理:将新鲜叠鞘石斛去除叶片,放入清洗液中浸泡清洗8min,然后捞出送到脱水机中脱除其表面的水分,备用:
(2)烘干:将脱水后的叠鞘石斛送到热风循环烘箱中,在50-60℃下烘干至含水量为60-70%后,切成石斛片;
(3)冷冻处理:将石斛片在-18℃下冷冻15h;
(4)压差膨化处理:将冷冻石斛片添加到膨化罐内进行压差膨化,制得膨化石斛片;
(5)低温回流提取浓缩:将膨化石斛片添加到热回流低温提取低温浓缩机中,加入其质量10倍的有机溶剂低温回流提取浓缩9h,制得一次浓缩物;
(6)浓缩:将一次浓缩物送到球形真空浓缩罐中浓缩,制得二次浓缩物;
(7)干燥粉碎:将二次浓缩物送到高真空干燥机干燥后,再经无尘粉碎机粉碎至200-300目,制得粗叠鞘石斛粉;
(8)配料:将粗叠鞘石斛粉与其质量1-2%的微晶纤维素搅拌混合均匀,即得叠鞘石斛粉。
所述清洗液中含有1.2%肉桂酸、0.6%甘草素、1.5%抗坏血酸、4.5%大蒜素、3.2%植酸、0.152%氯化钙,其余为水。
所述压差膨化为:将膨化罐内的压力保持在0.05Pa,加热至60℃,保持该温度和压力20s,之后控制压力瞬间降低至-0.08MPa,即得膨化石斛片。
所述步骤(5)的膨化石斛片低温回流提取前经经过了发酵处理,发酵处理的方法为:向膨化石斛片中加入其质量0.25%的石斛花精油,然后加入其质量0.012%的菌液在25-30℃发酵9h,灭菌后再进行低温回流提取。
所述菌液为解淀粉芽孢杆菌菌液,其活菌数为1-2×106cfu/ml。
所述步骤(5),有机溶剂为80%乙醇,低温回流提取浓缩的条件为:提取罐内压力0.03MPa,罐内温度55-80℃,浓缩比重1.2-1.35。
实施例3
一种叠鞘石斛粉的制备方法,包括以下步骤:
(1)清洗处理:将新鲜叠鞘石斛去除叶片,放入清洗液中浸泡清洗8min,然后捞出送到脱水机中脱除其表面的水分,备用:
(2)烘干:将脱水后的叠鞘石斛送到热风循环烘箱中,在50-60℃下烘干至含水量为60-70%后,切成石斛片;
(3)冷冻处理:将石斛片在-18℃下冷冻20h;
(4)压差膨化处理:将冷冻石斛片添加到膨化罐内进行压差膨化,制得膨化石斛片;
(5)低温回流提取浓缩:将膨化石斛片添加到热回流低温提取低温浓缩机中,加入其质量10倍的有机溶剂低温回流提取浓缩10h,制得一次浓缩物;
(6)浓缩:将一次浓缩物送到球形真空浓缩罐中浓缩,制得二次浓缩物;
(7)干燥粉碎:将二次浓缩物送到高真空干燥机干燥后,再粉碎至200-300目,制得粗叠鞘石斛粉;
(8)配料:将粗叠鞘石斛粉与其质量1.2%的微晶纤维素搅拌混合均匀,即得叠鞘石斛粉。
所述清洗液中含有2%肉桂酸、1%甘草素、2%抗坏血酸、5%大蒜素、4%植酸、0.2%氯化钙,其余为水。
所述压差膨化为:将膨化罐内的压力保持在0.05Pa,加热至60℃,保持该温度和压力20s,之后控制压力瞬间降低至-0.08MPa,即得膨化石斛片。
所述步骤(5)的膨化石斛片低温回流提取前经经过了发酵处理,发酵处理的方法为:向膨化石斛片中加入其质量0.15%的石斛花精油,然后加入其质量0.02%的菌液在25-30℃发酵10h,灭菌后再进行低温回流提取。
所述菌液为解淀粉芽孢杆菌菌液,其活菌数为1-2×106cfu/ml。
所述步骤(5),有机溶剂为80%乙醇,低温回流提取浓缩的条件为:提取罐内压力0.03MPa,罐内温度55-80℃,浓缩比重1.2-1.35。
实施例4
一种叠鞘石斛粉的制备方法,包括以下步骤:
(1)清洗处理:将新鲜叠鞘石斛去除叶片,放入清洗液中浸泡清洗8min,然后捞出送到脱水机中脱除其表面的水分,备用:
(2)烘干:将脱水后的叠鞘石斛送到热风循环烘箱中,在50-60℃下烘干至含水量为60-70%后,切成石斛片;
(3)冷冻处理:将石斛片在-18℃下冷冻20h;
(4)压差膨化处理:将冷冻石斛片添加到膨化罐内进行压差膨化,制得膨化石斛片;
(5)低温回流提取浓缩:将膨化石斛片添加到热回流低温提取低温浓缩机中,加入其质量10倍的有机溶剂低温回流提取浓缩10h,制得一次浓缩物;
(6)浓缩:将一次浓缩物送到球形真空浓缩罐中浓缩,制得二次浓缩物;
(7)干燥粉碎:将二次浓缩物送到高真空干燥机干燥后,再经无尘粉碎机粉碎至200-300目,制得粗叠鞘石斛粉;
(8)配料:将粗叠鞘石斛粉与其质量1.2%的微晶纤维素搅拌混合均匀,即得叠鞘石斛粉。
所述清洗液中含有2%肉桂酸、1%甘草素、2%抗坏血酸、5%大蒜素、4%植酸、0.2%氯化钙,其余为水。
所述压差膨化为:将膨化罐内的压力保持在0.05Pa,加热至60℃,保持该温度和压力20s,之后控制压力瞬间降低至-0.08MPa,即得膨化石斛片。
所述步骤(5),有机溶剂为80%乙醇,低温回流提取浓缩的条件为:提取罐内压力0.03MPa,罐内温度55-80℃,浓缩比重1.2-1.35。
对比例1
对比例1与实施例1的区别在于采用的清洗液是纯水。
对比例2
对比例2与实施例1的区别在于没有压差膨化处理过程。
对比例3
对比例3与实施例1的区别在于没有冷冻处理过程。
对比例4
对比例4与实施例1的区别在于没有采用辅料微晶纤维素进行配料。
试验例1
对本发明实施例和对比例1-4的制备叠鞘石斛粉进行性能测定,结果如表1所示:
表1
在此有必要指出的是,以上实施例和试验例仅限于对本发明的技术方案做进一步的阐述和理解,不能理解为对本发明的技术方案做进一步的限定,本领域技术人员作出的非突出实质性特征和显著进步的发明创造,仍然属于本发明的保护范畴。
Claims (6)
1.一种叠鞘石斛粉的制备方法,其特征在于,包括以下步骤:
(1)清洗处理:将新鲜叠鞘石斛去除叶片,放入清洗液中浸泡清洗6-8min,然后捞出送到脱水机中脱除其表面的水分,备用;
所述清洗液中含有1-2%肉桂酸、0.5-1%甘草素、1-2%抗坏血酸、4-5%大蒜素、3-4%植酸、0.1-0.2%渗透压调节剂,其余为水;
(2)烘干:将脱水后的叠鞘石斛送到热风循环烘箱中,在50-60℃下烘干至含水量为60-70%后,切成片状,制得石斛片;
(3)冷冻处理:将石斛片在15℃~-18℃下冷冻15-20h;
(4)压差膨化处理:将冷冻石斛片添加到膨化罐内进行压差膨化,制得膨化石斛片;
(5)低温回流提取浓缩:将膨化石斛片添加到热回流低温提取低温浓缩机中,加入其质量8-10倍有机溶剂低温回流提取浓缩8-10h,制得一次浓缩物;
(6)浓缩:将一次浓缩液送到球形真空浓缩罐中浓缩,制得二次浓缩物;
(7)干燥粉碎:将二次浓缩物送到高真空干燥机干燥后,再经无尘粉碎机粉碎至200-300目,制得粗叠鞘石斛粉;
(8)配料:将粗叠鞘石斛粉与其质量1-2%的辅料搅拌混合均匀,即得叠鞘石斛粉;
所述步骤(5)的膨化石斛片低温回流提取前经过了发酵处理,发酵处理的方法为:向膨化石斛片中加入其质量0.1-0.15%的石斛花精油,然后加入其质量0.01-0.02%的菌液在25-30℃发酵8-10h,灭菌后再进行低温回流提取。
2.如权利要求1所述的叠鞘石斛粉的制备方法,其特征在于,所述渗透压调节剂为氯化钙。
3.如权利要求1所述的叠鞘石斛粉的制备方法,其特征在于,所述压差膨化为:将膨化罐内的压力保持在0.05Pa,加热至60℃,保持该温度和压力20s,之后控制压力瞬间降低至-0.08MPa,即得膨化石斛片。
4.如权利要求1所述的叠鞘石斛粉的制备方法,其特征在于,所述菌液为解淀粉芽孢杆菌菌液,其活菌数为1-2×106cfu/ml。
5.如权利要求1所述的叠鞘石斛粉的制备方法,其特征在于,所述步骤(5),有机溶剂为80%乙醇,低温回流提取浓缩的条件为:提取罐内压力0.03MPa,罐内温度55-80℃,浓缩比重1.2-1.35。
6.如权利要求1所述的叠鞘石斛粉的制备方法,其特征在于,所述步骤(8),辅料为微晶纤维素。
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