CN113456770A - 一种强力枇杷露及其制备方法 - Google Patents
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Abstract
本发明提供一种强力枇杷露及其制备方法,包括如下步骤:(1)将药材加入水,煮沸,过滤,加水重复煮沸,过滤,合并滤液,得水提液;(2)将水提液经大孔树脂后进行梯度洗脱,合并洗脱液,得粗提液;(3)在蔗糖中加入水,控制蒸汽压力进行熬煮,冷却,加入蔗糖酶酶解,得酶解液;(4)在粗提液中加入酶解液,加热,冷藏后,取上清液,浓缩处理,得药膏;(5)在药膏中加入苯甲酸钠,煮沸,后续进行调配,得成品。本发明制得的强力枇杷露不仅出膏率高,同时还有较高的药效成分,且放置较长时间产品的稳定性保持较好,本发明的生产工艺简单、设备要求较低,产品质量易于控制,可实现强力枇杷露的大规模工业生产。
Description
技术领域
本发明涉及中药制药领域,特别涉及一种强力枇杷露及其制备方法。
背景技术
强力枇杷露,为淡棕色澄清液体,具有养阴敛肺,止咳祛痰的作用,可用于支气管炎咳嗽。在枇杷露的基础上加入罂粟壳,罂粟壳因可抑制呼吸道腺体分泌及纤毛运动,对剧烈干咳及刺激性咳嗽具有较好地抑制作用,因此形成强力枇杷露。但强力枇杷露在制备的过程中,药液经过浓缩形成的药膏,稠度大容易阻碍后续辅料的加入,使辅料与药膏相容性变差,导致出膏率低,且造成成品不稳定,易产生沉淀,进而影响产品的质量与治疗效果。
申请号CN109125258B公开了一种强力枇杷露的制备工艺,将中药煎煮液进行浓缩、澄清后,采用阳离子交换树脂、硅胶树脂、固相萃取小柱和色谱法进行多次富集,最后将富集液煎煮和配制得到成品;现有技术采用多种化学试剂进行多步富集的提取纯化方式,难以保证化学试剂的残留量以及成品在存放过程中与药效成分的反应和影响,同时工艺较为复杂、设备要求较高和成本相应提高,不利于现代制药业的大规模应用。申请号CN106620452A公开了一种强力枇杷露的制备工艺,将中药煎煮液进行过滤浓缩,采用包合物将浓缩液进行包合,经调配得到成品。现有技术通常都是在调配时加入蔗糖进行熬煮,一方面易使溶液变稠,影响辅料的溶解性,另一方面,蔗糖在熬煮时容易爆沸和焦化,生产不安全,同时产品质量不易控制。
发明内容
鉴以此,本发明的目的在于提出一种强力枇杷露及其制备方法,提高出膏率和药效成分,增加强力枇杷露的稳定性,使生产工艺简单、产品质量可控、设备要求较低,可实现强力枇杷露的大规模工业生产。
本发明的技术方案是这样实现的:
一种强力枇杷露,包括如下的药材:枇杷叶、罂粟壳、百部、白前、桔梗、桑白皮、苯甲酸钠、蔗糖、枸橼酸、薄荷香精、薄荷脑的重量比为69:50:15:9:6:6:2.5:600:0.5:0.25:0.15。
该强力枇杷露的制备方法,包括如下步骤:
(1)水提液:将枇杷叶置于底部,依次加入桑白皮、罂粟壳、百部、白前和桔梗混合,加入水,料液重量比为1:7~9;煮沸1.5~2.5h,过滤,加水重复煮沸2-3次,过滤,合并滤液,得水提液;
(2)粗提液:将水提液经大孔树脂进行吸附处理,水提液经大孔树脂的体积流量1.5~2.5mL/min,依次采用2~4倍柱体积的质量浓度45~55%乙醇溶液和2~4BV质量浓度65~75%乙醇溶液进行梯度洗脱,合并洗脱液,得粗提液;
其中,树脂使用前进行前处理,前处理方法包括如下步骤:
(a)在树脂中加入无水乙醇溶液至浸没树脂,浸泡16~18h后,依次采用2~4倍柱体积的无水乙醇溶液和2~4倍柱体积的去离子水洗脱树脂,得预处理树脂1;
(b)在所述预处理树脂1中加入1.5~2.5倍柱体积的质量浓度30~40%乙醇溶液,浸泡3~4h后,以体积流量5~6BV/h进行洗脱,得预处理树脂2;
(c)取所述预处理树脂2,采用去离子水洗脱至洗脱液呈中性后,加入2~4倍柱体积的质量浓度60~70%乙醇溶液进行洗脱,最后采用去离子水洗脱至洗脱液呈中性;
(3)酶解液:在蔗糖中加入3~4倍重量的水,得蔗糖水溶液,控制蒸汽压力0.08~0.12MPa,煮至固形物浓度至60~70%时,停止熬煮,冷却,加入蔗糖酶,酶解得酶解液;蔗糖酶与蔗糖水溶液的质量比为0.002~0.004:1;
进一步说明,酶解为于35~55℃水浴保温6~8h;
(4)药膏:在粗提液中加入酶解液,加热,于5~10℃冷藏12~14h,取上清液,于70~80℃浓缩至相对密度1.06~1.10,得药膏;加入苯甲酸钠,搅拌至溶解,静置2.5~3.5h,粗提液和酶解液的质量比为1:0.6~0.7;
进一步说明,加热是以升温速率50~60℃/min升温至100~110℃;
(5)成品:在药膏中加入苯甲酸钠,搅拌至溶解,煮沸15~25min,静置2.5~3.5h,冷却过滤后,加入枸橼酸、薄荷香精和薄荷脑混匀,静置2.5~3.5h,过滤,得半成品溶液,加入水,搅拌25~35min,过滤,得成品;半成品溶液与水的质量比为1:1。
与现有技术相比,本发明的有益效果为:
本发明通过采用逐级纯化中药材水提液的方式,不仅提高药材中有效成分的含量,还可降低浓缩时形成药膏的稠度,从而增加辅料与药膏的相容性,并进一步提高药膏的出膏率,提高产品质量的稳定性。
本发明采用大孔树脂吸附结合蔗糖酶解液处理中药水提取液,一方面利用树脂有机高聚物吸附的特性,可起到分离纯化药效成分的作用,另一方面利用蔗糖经酶解后含有多种小分子糖的溶液,先加入中药水提取液中,不仅可降低溶液的粘稠度,有利于增大后续辅料与药膏的融合性,还可防止糖液在熬煮过程中发生爆沸溢出或焦化的现象,并减少人体对蔗糖过多的摄入,同时经过树脂吸附处理的药材提取液,可使分子和分子相互作用获得弱性的非共价键合作用,从而增加药物分子与小分子糖分子的作用力,提高溶液的稳定性。
另外,本发明采用低温冷藏处理,可进一步去除粗提液的部分杂质,能够有效提高中药提取液的药物成分,冷藏前进行快速加热和冷藏期间的低温,可使溶液形成强烈的温差,加速分子的运动,促使药物分子与小分子糖分子的分子间进行重新排列,增加药物分子和小分子糖分子的分子间作用力,可减少后续调配加热过程中分子结构的破坏,进一步提高药膏的稳定程度。
具体实施方式
为了更好理解本发明技术内容,下面提供具体实施例,对本发明做进一步的说明。
本发明实施例所用的实验方法如无特殊说明,均为常规方法。
本发明实施例所用的材料、试剂等,如无特殊说明,均可从商业途径得到。
实施例1
一种强力枇杷露,包括如下重量的中药材:
按重量比为69:50:15:9:6:6:2.5:600:0.5:0.25:0.15,称取枇杷叶69g、罂粟壳50g、百部15g、白前9g、桔梗6g、桑白皮6g、苯甲酸钠2.5g、蔗糖600g、枸橼酸0.5g、薄荷香精0.25g、薄荷脑0.15g;
该强力枇杷露的制备步骤如下:
(1)水提液:将枇杷叶置于底部,依次加入桑白皮、罂粟壳、百部、白前和桔梗混合,加入7倍重量的水,煮沸1.5h,过滤,加水重复煮沸2次,过滤,合并滤液,得水提液;
(2)粗提液:将水提液经大孔树脂进行吸附处理,水提液经大孔树脂的体积流量1.5mL/min,依次采用2倍柱体积的质量浓度45%乙醇溶液、2倍柱体积的质量浓度65%乙醇溶液进行梯度洗脱,合并洗脱液,得粗提液;其中,树脂使用前的前处理方法包括如下步骤:
(a)在树脂中加入无水乙醇溶液至浸没树脂,浸泡16h后,依次采用2倍柱体积的无水乙醇溶液和3倍柱体积的去离子水洗脱树脂,得预处理树脂1;
(b)在预处理树脂1中加入1.5倍柱体积的质量浓度30%乙醇溶液,浸泡3h后,以体积流量5BV/h进行洗脱,得预处理树脂2;
(c)取预处理树脂2,采用去离子水洗脱至洗脱液呈中性后,加入2倍柱体积的质量浓度70%乙醇溶液进行洗脱,最后采用去离子水洗脱至洗脱液呈中性。
(3)酶解液:在蔗糖中加入3倍重量的水,得蔗糖水溶液,控制蒸汽压力0.08MPa,煮至固形物浓度至60%时,停止熬煮,冷却,按蔗糖酶与蔗糖水溶液的质量比为0.002:1,加入蔗糖酶,于35℃水浴保温6h进行酶解,得酶解液;
(4)药膏:按质量比为1:0.6,取粗提液500g,加入酶解液,以升温速率50℃/min升温至100℃进行加热,于5℃冷藏12h,取上清液,于70℃浓缩至相对密度为1.10,得药膏;
(5)成品:在药膏中加入苯甲酸钠,搅拌至溶解,煮沸15min,静置2.5h,冷却过滤后,加入枸橼酸、薄荷香精和薄荷脑混匀,静置2.5h,过滤,得半成品溶液,按质量比为1:1,在半成品溶液中加入水,搅拌25min,过滤,得成品。
实施例2
根据实施例1的强力枇杷露的相同配方,该强力枇杷露的制备步骤如下:
(1)水提液:将枇杷叶置于底部,依次加入桑白皮、罂粟壳、百部、白前和桔梗混合,加入9倍重量的水,煮沸2.5h,过滤,加水重复煮沸3次,过滤,合并滤液,得水提液;
(2)粗提液:将水提液经大孔树脂进行吸附处理,水提液经大孔树脂的体积流量2.5mL/min,依次采用4倍柱体积的质量浓度45%乙醇溶液、4倍柱体积的质量浓度65%乙醇溶液进行梯度洗脱,合并洗脱液,得粗提液;其中,树脂使用前的前处理方法包括如下步骤:
(a)在树脂中加入无水乙醇溶液至浸没树脂,浸泡18h后,依次采用4倍柱体积的无水乙醇溶液和4倍柱体积的去离子水洗脱树脂,得预处理树脂1;
(b)在预处理树脂1中加入2.5倍柱体积的质量浓度40%乙醇溶液,浸泡4h后,以体积流量6BV/h进行洗脱,得预处理树脂2;
(c)取所述预处理树脂2,采用去离子水洗脱至洗脱液呈中性后,加入4倍柱体积的质量浓度60%乙醇溶液进行洗脱,最后采用去离子水洗脱至洗脱液呈中性。
(3)酶解液:在蔗糖中加入3倍重量的水,得蔗糖水溶液,控制蒸汽压力0.12MPa,煮至固形物浓度至70%时,停止熬煮,冷却,按蔗糖酶与蔗糖水溶液的质量比为0.004:1,加入蔗糖酶,于55℃水浴保温8h进行酶解,得酶解液;
(4)药膏:按质量比为1:0.7,取粗提液500g,加入酶解液,以升温速率60℃/min升温至110℃进行加热,于10℃冷藏14h,取上清液,于80℃浓缩至相对密度为1.06,得药膏;
(5)成品:在药膏中加入苯甲酸钠,搅拌至溶解,煮沸25min,静置3.5h,冷却过滤后,加入枸橼酸、薄荷香精和薄荷脑混匀,静置3.5h,过滤,得半成品溶液,按质量比为1:1,在半成品溶液中加入水,搅拌35min,过滤,得成品。
实施例3
根据实施例1的强力枇杷露的相同配方,该强力枇杷露的制备步骤如下:
(1)水提液:将枇杷叶置于底部,依次加入桑白皮、罂粟壳、百部、白前和桔梗混合,加入8倍重量的水,煮沸2h,过滤,加水重复煮沸2次,过滤,合并滤液,得水提液;
(2)粗提液:将水提液经大孔树脂进行吸附处理,水提液经大孔树脂的体积流量2.0mL/min,依次采用3倍柱体积的质量浓度45%乙醇溶液、3倍柱体积的质量浓度65%乙醇溶液进行梯度洗脱,合并洗脱液,得粗提液;其中,树脂使用前的前处理方法包括如下步骤:
(a)在树脂中加入无水乙醇溶液至浸没树脂,浸泡17h后,依次采用3倍柱体积的无水乙醇溶液和4倍柱体积的去离子水洗脱树脂,得预处理树脂1;
(b)在预处理树脂1中加入2倍柱体积的质量浓度35%乙醇溶液,浸泡3.5h后,以体积流量6BV/h进行洗脱,得预处理树脂2;
(c)取预处理树脂2,采用去离子水洗脱至洗脱液呈中性后,加入3倍柱体积的质量浓度65%乙醇溶液进行洗脱,最后采用去离子水洗脱至洗脱液呈中性。
(3)酶解液:在蔗糖中加入3倍重量的水,得蔗糖水溶液,控制蒸汽压力0.10MPa,煮至固形物浓度至65%时,停止熬煮,冷却,按蔗糖酶与蔗糖水溶液的质量比为0.003:1,加入蔗糖酶,于45℃水浴保温7h进行酶解,得酶解液;
(4)药膏:按质量比为1:0.65,取粗提液500g,加入酶解液,以升温速率55℃/min升温至110℃进行加热,于8℃冷藏13h,取上清液,于75℃浓缩至相对密度为1.08,得药膏;
(5)成品:在药膏中加入苯甲酸钠,搅拌至溶解,煮沸20min,静置3h,冷却过滤后,加入枸橼酸、薄荷香精和薄荷脑混匀,静置3h,过滤,得半成品溶液,按质量比为1:1,在半成品溶液中加入水,搅拌30min,过滤,得成品。
对比例1
根据实施例3的强力枇杷露的相同配方,其区别在于:树脂前处理方法不同,即,在树脂中加入无水乙醇溶液至浸没树脂,浸泡20h后,以体积流量3BV/h,采用5倍柱体积的质量浓度65%乙醇溶液进行洗脱,去离子水洗脱至洗脱液呈中性。
对比例2
根据实施例3的强力枇杷露的相同配方,其区别在于:粗提液的制备方法不同,即,将水提液经大孔树脂进行吸附处理,水提液经大孔树脂的体积流量5.5mL/min,依次采用6倍柱体积的质量浓度80%乙醇溶液和5倍柱体积的质量浓度50%乙醇溶液进行洗脱,合并洗脱液,得粗提液。
对比例3
根据实施例3的强力枇杷露的相同配方,其区别在于:酶解液的制备方法不同,即,在蔗糖中加入3倍重量的水,得蔗糖水溶液,控制蒸汽压力0.20MPa,煮至固形物浓度至40%时,停止熬煮,冷却,按蔗糖酶与蔗糖水溶液的质量比为0.005:1,加入蔗糖酶,于45℃水浴保温7h进行酶解,得酶解液。
对比例4
根据实施例3的强力枇杷露的相同配方,其区别在于:步骤(4)加热和冷藏条件不同,即,在粗提液中加入酶解液,以升温速率30℃/min升温至80℃进行加热,于15℃冷藏13h;其余步骤同实施例3。
对比例5
根据实施例3的强力枇杷露的相同配方,其区别在于:采用传统煮糖工艺替代蔗糖酶解工艺,包括如下制备步骤:
(1)水提液:将枇杷叶置于底部,依次加入桑白皮、罂粟壳、百部、白前和桔梗混合,加入8倍重量的水,煮沸2h,过滤,加水重复煮沸2次,过滤,合并滤液,得水提液;
(2)粗提液:将水提液经大孔树脂进行吸附处理,水提液经大孔树脂的体积流量2.0mL/min,依次采用3倍柱体积的质量浓度45%乙醇溶液、3倍柱体积的质量浓度65%乙醇溶液进行梯度洗脱,合并洗脱液,得粗提液;其中,树脂使用前的前处理方法包括如下步骤:
(a)在树脂中加入无水乙醇溶液至浸没树脂,浸泡17h后,依次采用3倍柱体积的无水乙醇溶液和4倍柱体积的去离子水洗脱树脂,得预处理树脂1;
(b)在预处理树脂1中加入2倍柱体积的质量浓度35%乙醇溶液,浸泡3.5h后,以体积流量6BV/h进行洗脱,得预处理树脂2;
(c)取预处理树脂2,采用去离子水洗脱至洗脱液呈中性后,加入3倍柱体积的质量浓度65%乙醇溶液进行洗脱,最后采用去离子水洗脱至洗脱液呈中性。
(3)药膏:将粗提液以升温速率55℃/min升温至110℃进行加热,于8℃冷藏13h,取上清液,于75℃浓缩至相对密度为1.08,得药膏;
(4)成品:在药膏中加入苯甲酸钠和蔗糖,搅拌至溶解,控制蒸汽压力0.10MPa,煮沸20min,静置3h,冷却过滤后,加入枸橼酸、薄荷香精和薄荷脑混匀,静置3h,过滤,得半成品溶液,按质量比为1:1,在半成品溶液中加入水,搅拌30min,过滤,得成品。
一、实验测试
实验方法:根据《中国药典》2020年版,采用日本岛津GC-17A气相色谱仪测定薄荷脑含量,采用日本岛津LC-2010HT高效液相色谱仪测定可待因含量;分别采用实施例1~3和对比例1~5的制备方法,制备三批强力枇杷露,于温度30℃±2℃、相对湿度65%±5%、避光通风的条件下进行稳定性实验,分别测定0个月末和放置6个月末的薄荷脑和可待因含量,同时观察放置9个月末的产品外观性状,选用市售的强力枇杷露(广西恒科药业,国药准字Z20053763,规格:180mL/瓶)作为对照品,药膏出膏率(%)=(清膏重量/药材总重量)×100%,测定结果如表1:
由上表可知,本发明实施例1~3制备的强力枇杷露,出膏率在68%以上,薄荷脑和可待因的含量分别在0.0252mg/mL和12.82mg/mL以上,放置6个月末薄荷脑和可待因的含量损失较少,同时放置9个月末时,产品呈现淡棕色的澄清液体,表明本发明采用大孔树脂吸附处理结合蔗糖酶解液和低温冷藏的工艺,可提高出膏率、薄荷脑和可待因含量,进一步提高产品的治疗效果和质量的稳定性。实施例4改变了药材水提取液的体积流量,薄荷脑和可待因的含量稍有降低,控制一定的药材水提取液有利于树脂充分地分离纯化提取液中的药效成分。
对比例1~5出膏率在59.2~66.4%之间,放置6个月末产品的薄荷脑和可待因含量下降较快,与0个月末相比,薄荷脑含量下降最高达到23.3%,可待因最高为7.5%;对比例2的薄荷脑含量稍有降低,成品出现较澄清的现象,表明经过特定工艺的乙醇梯度洗脱程序,不仅可提高成品中薄荷脑的含量,同时提高产品的稳定性;对比例3的酶解液制备不同,溶液中固形物含量不同,酶解生成的小分子种类和含量有所不同,进而影响后续成品稳定性的问题;对比例4和对比例5放置9个末,产品出现轻微浑浊的现象,对比例5较严重,产品颜色变深,表明传统煮糖工艺使蔗糖分子在熬煮过程中容易产生焦化现象,并留存有部分残渣,易使产品在长期放置的过程中出现不稳定的现象。
综上所述,本发明采用大孔树脂吸附、酶解蔗糖和低温冷藏,结合特定的制备工艺,不仅提高产品的出膏率,还可提高强力枇杷露中的薄荷脑和可待因含量,且降低薄荷脑和可待因含量的损失量,进一步提高产品在长时间放置下的稳定性,有利于稳定和控制产品的质量,提升产品的治疗效果。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (10)
1.一种强力枇杷露的制备方法,其特征在于:包括如下步骤:
(1)水提液:将枇杷叶置于底部,依次加入桑白皮、罂粟壳、百部、白前和桔梗混合,加入水,料液重量比为1:7~9;煮沸1.5~2.5h,过滤,加水重复煮沸2-3次,过滤,合并滤液,得水提液;
(2)粗提液:将水提液经大孔树脂进行吸附处理,采用梯度洗脱,合并洗脱液,得粗提液;
(3)酶解液:在蔗糖中加入3~4倍重量的水,得蔗糖水溶液,控制蒸汽压力0.08~0.12MPa,煮至固形物浓度至60~70%时,停止熬煮,冷却,加入蔗糖酶,酶解得酶解液;
(4)药膏:在粗提液中加入酶解液,加热,于5~10℃冷藏12~14h,取上清液,于70~80℃浓缩至相对密度为1.06~1.10,得药膏;
(5)成品:在药膏中加入苯甲酸钠,搅拌至溶解,煮沸15~25min,静置2.5~3.5h,冷却过滤后,加入枸橼酸、薄荷香精和薄荷脑混匀,静置2.5~3.5h,过滤,得半成品溶液,加入水,搅拌25~35min,过滤,得成品。
2.如权利要求1的一种强力枇杷露的制备方法,其特征在于:所述枇杷叶、罂粟壳、百部、白前、桔梗、桑白皮、苯甲酸钠、蔗糖、枸橼酸、薄荷香精、薄荷脑的重量比为69:50:15:9:6:6:2.5:600:0.5:0.25:0.15。
3.如权利要求1的一种强力枇杷露的制备方法,其特征在于:所述树脂使用前进行前处理,前处理方法包括如下步骤:
(a)在树脂中加入无水乙醇溶液至浸没树脂,浸泡16~18h后,依次采用2~4倍柱体积的无水乙醇溶液和2~4倍柱体积的去离子水洗脱树脂,得预处理树脂1;
(b)在所述预处理树脂1中加入1.5~2.5倍柱体积的质量浓度30~40%乙醇溶液,浸泡3~4h后,以体积流量5~6BV/h进行洗脱,得预处理树脂2;
(c)取所述预处理树脂2,采用去离子水洗脱至洗脱液呈中性后,加入2~4倍柱体积的质量浓度60~70%乙醇溶液进行洗脱,最后采用去离子水洗脱至洗脱液呈中性。
4.如权利要求1的一种强力枇杷露的制备方法,其特征在于:所述水提液经大孔树脂的体积流量1.5~2.5mL/min。
5.如权利要求1的一种强力枇杷露的制备方法,其特征在于:所述梯度洗脱为依次采用2~4倍柱体积的质量浓度45~55%乙醇溶液和2~4倍柱体积的质量浓度65~75%乙醇溶液进行洗脱。
6.如权利要求1的一种强力枇杷露的制备方法,其特征在于:所述蔗糖酶与蔗糖水溶液的质量比为0.002~0.004:1。
7.如权利要求1的一种强力枇杷露的制备方法,其特征在于:所述酶解为于35~55℃水浴保温6~8h。
8.如权利要求1的一种强力枇杷露的制备方法,其特征在于:步骤(4)中,所述粗提液和酶解液的质量比为1:0.6~0.7。
9.如权利要求1的一种强力枇杷露的制备方法,其特征在于:步骤(4)中,所述加热是以升温速率50~60℃/min升温至100~110℃。
10.如权利要求1的一种强力枇杷露的制备方法,其特征在于:步骤(5)中,所述半成品溶液与水的质量比为1:1。
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