CN103550065B - 一种复合挤出法生产淀粉基软胶囊的方法 - Google Patents
一种复合挤出法生产淀粉基软胶囊的方法 Download PDFInfo
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Abstract
本发明公开了一种淀粉基胶囊的制备方法,具体是将淀粉预混物料和凝胶剂分别挤出成膜,再经多层共挤机复合成复合淀粉膜,再将所述复合淀粉膜经旋转冲膜法制成淀粉基软胶囊。
Description
技术领域
本发明涉及到软胶囊的制备方法,具体是一种非明胶软胶囊的制备方法。
背景技术
胶囊一般用于包裹不宜直接与食道接触,需要在胃或肠道中再崩解作用的药物。目前大部分药用或保健食品的胶囊是由明胶制成,明胶来自于动物的皮或骨,经酸或碱处理,熬制而得。其生产过程中,不可避免的会有动物蛋白残留,会和内容药物产生相互作用,从而导致药物变质等不良后果。
此外,动物来源的明胶,对于素食主义者以及持有***、犹太等宗教信仰的人士是无法接受的。同样的,对于过敏体质的人群,也是应当避免摄入明胶制品。
淀粉是植物来源,其来源广泛且量大,价格要远低于明胶。经改性的淀粉将获得更好的凝胶能力和机械强度,使其接近明胶的性质。利用淀粉制作软胶囊,将克服现有明胶胶囊的种种缺陷,同时具有成本低廉的优势,值得推广应用。
在现有技术中,淀粉胶囊的制备方法大多如下:预先制备好淀粉凝胶液,再送入胶囊机中,使用模具或者沾胶成型。在软胶囊的制备中,将胶液涂覆在模具上,形成具有凹槽的薄片,经装料、辊筒压合后封包成软胶囊。上述的技术,虽具有操作简便的优势,但生产的胶囊包封性能不佳,涂覆膜层厚度不均,影响胶囊质量。
本发明方案中,采用挤出机分别制备淀粉基挤出膜和凝胶剂挤出膜,再经多层共挤机将二者共同挤出成为一体,能确保凝胶剂挤出膜的均一,并大大增强胶囊壳的封包性能。
发明内容
本发明公开了一种淀粉软胶囊的制备方法,包含以下步骤:
(1)复合淀粉膜的制备:由淀粉、抗结剂和糊化剂预混制成淀粉基预混物料,经挤出机制成淀粉基挤出膜;再将凝胶剂、水分保持剂和乳化剂溶于水制成凝胶剂糊液,经挤出机制成凝胶剂挤出膜,将凝胶剂挤出膜复合在淀粉挤出膜上经共挤制成复合淀粉膜,膜的厚度为0.2-1mm,拉伸模量大于3MPa,断裂伸长率为80%-140%;
(2)淀粉基软胶囊的制备:将两张复合淀粉膜,经旋转冲模法制成淀粉基软胶囊。
具体包含如下步骤:
(1)复合淀粉膜的制备
复合淀粉膜是由淀粉与凝胶剂经复合法制备而成。
所述复合法,具体如下:
(a)将淀粉和抗结剂放入高速混合机下以1500-2000rpm的转速,60℃下混合2min后搅拌混合,再将糊化剂在搅拌下缓缓加入高速混合机中,继续混合5min制成淀粉基预混物料。
(b)将淀粉基预混物料投入双螺杆挤出机,把混合后的物料挤出造粒得到淀粉基粒料,使用单螺杆挤出机。把淀粉基粒料制成膜,得到淀粉基挤出膜。
(c)将凝胶剂、水分保持剂和乳化剂溶于水得凝胶剂糊液,投入单螺杆挤出机制成凝胶剂挤出膜。
(d)将凝胶剂挤出膜置于多层共挤机上层辊筒,淀粉基挤出膜置于下层辊筒,通过共挤模口制成复合淀粉膜。
在上述步骤(a)中,所述淀粉为各种天然来源的淀粉,或经物理、化学手段改性的天然来源淀粉。优选酯化的木薯淀粉。
在上述步骤(a)中,所述抗结剂为药用级硬脂酸或脂肪酸甘油酯。
在上述步骤(a)中,所述糊化剂为去离子水。
在上述步骤(b)中,所述双螺杆挤出参数为:物料温度在25-170℃之间,螺杆转速60-400转/分钟。优选60-160℃,100-150℃,70℃,80℃,90℃,100℃,120℃,130℃,140℃。
在上述步骤(b)中,所述单螺杆挤出参数为:物料温度在25-170℃之间,螺杆转速60-400转/分钟。优选60-160℃,100-150℃,70℃,80℃,90℃,100℃,120℃,130℃,140℃。
在上述步骤(c)中,所述凝胶剂,为支链淀粉、结冷胶、卡拉胶、黄原胶、瓜尔胶或各种植物胶的一种或多种组合。
在上述步骤(c)中,所述乳化剂为离子型乳化剂,优选药用级十二烷基硫酸的碱金属盐或十二烷基磺酸的碱金属盐,如药用级十二烷基硫酸钠或十二烷基磺酸钠。
在上述步骤(c)中,所述水分保持剂为药用级甘油或药用级山梨糖醇。
在上述步骤(c)中,所述单螺杆挤出机参数为:物料温度在25-110℃之间,螺杆转速60-300转/分钟。优选50-160℃,100-150℃,70℃,80℃,90℃,100℃,120℃,130℃,140℃,
在上述步骤(d)中,组成复合淀粉膜的凝胶剂挤出膜与淀粉基挤出膜单位面积的重量比为1:10-1:20。
在上述步骤(d)中,复合淀粉膜的厚度为0.2-1mm,拉伸模量大于3MPa,断裂伸长率为80%-140%。
(2)淀粉基软胶囊的制备
淀粉基软胶囊采用旋转冲模法制备,具体如下:
将两张复合淀粉膜,各自经辊筒送入旋转冲模机的两个紧挨的圆筒模具,需注意附有凝胶剂挤出膜的一面应朝上。调节模具温度为40-90℃,开动机器,两个圆筒模具异向向内带动两张复合淀粉膜转动,模具上的凹槽可抽真空,使贴合在模具上的复合淀粉膜因真空而形成凹陷,再经模具的挤压形成具有空腔的软胶囊。在软胶囊成型同时,从两个圆筒模具结合处的正上方添加胶囊内容物。
需说明的是,凝胶剂挤出膜和淀粉基挤出膜并非简单的层结构叠加。使用本发明方案制备的复合淀粉膜做成的淀粉软胶囊,其封包性、稳定性更优,具有突出的进步性。
根据本发明所述方法制备的淀粉基软胶囊可以用于制备药品、保健品和功能食品。
具体实施例:
以下将列举数个实施实例,来进一步说明本发明内容及依据本发明方案生产的产品性质。所有实施例中,软胶囊的包容物为鱼肝油250mg。
实施例1
淀粉基挤出膜所用原料与重量比例如下:
淀粉:玉米淀粉,85%;
抗结剂:药用级硬脂酸,1.2%;
糊化剂:去离子水,13.8%。
凝胶剂挤出膜所用原料与重量比例如下:
凝胶剂:瓜尔胶,70%;
水分保持剂:药用级甘油,20%;
乳化剂:药用级十二烷基硫酸钠,2%;
去离子水:8% 。
复合法步骤如下:
(a)将淀粉和抗结剂放入高速混合机下以1500-2000rpm的转速,60℃下混合2min后搅拌混合,再将糊化剂在搅拌下缓缓加入高速混合机中,继续混合5min制成淀粉基预混物料。
(b)将淀粉基预混物料投入双螺杆挤出机,把混合后的物料挤出造粒得到淀粉基粒料,使用单螺杆挤出机。把淀粉基粒料制成膜,得到淀粉基挤出膜。
(c)将凝胶剂、水分保持剂和乳化剂溶于水得凝胶剂糊液,投入单螺杆挤出机制成凝胶剂挤出膜。
(d)将凝胶剂挤出膜置于多层共挤机上层辊筒,淀粉基挤出膜置于下层辊筒,通过共挤模口制成复合淀粉膜。
淀粉基胶囊制备步骤为:将复合膜放入加有温控的旋转冲模中制备出淀粉基胶囊,模具温度60℃。
步骤(b)中双螺杆挤出机参数如下:
在螺杆的转动速度为350转/分钟的条件下挤出,其中各滑块设定的温度为:
滑块1: 25℃
滑块2-3: 110℃
滑块4-6: 145℃
滑块7-9: 165℃
滑块10-12: 160℃
喷嘴: 160℃
步骤(b)中单螺杆挤出机的参数如下:
在螺杆的转动速度为350转/分钟的条件下挤出,设定的温度为160℃。
步骤(c)中单螺杆挤出机的参数如下:
在螺杆的转动速度为300转/分钟的条件下挤出,设定温度为105℃。
组成复合淀粉膜的凝胶剂挤出膜与淀粉基挤出膜的单位面积重量比为1:15,制成的复合淀粉膜厚度为0.5mm。
实施例2
淀粉基挤出膜所用原料与重量比例如下:
淀粉:绿豆淀粉,85%;
抗结剂:药用级硬脂酸,1.2%;
糊化剂:去离子水,13.8%。
凝胶剂挤出膜所用原料与重量比例如下:
凝胶剂:卡拉胶,70%;
水分保持剂:药用级甘油,20%;
乳化剂:药用级十二烷基硫酸钠,2%;
去离子水:8%。
其余同实施例1,组成复合淀粉膜的凝胶剂挤出膜与淀粉基挤出膜的单位面积重量比为1:14.7,制成的复合淀粉膜厚度为0.5mm。
实施例3
淀粉基挤出膜所用原料与重量比例如下:
淀粉:木薯淀粉,85%;
抗结剂:药用级硬脂酸,1.2%;
糊化剂:去离子水,13.8%。
凝胶剂挤出膜所用原料与重量比例如下:
凝胶剂:交联木薯胶,70%;
水分保持剂:药用级甘油,20%;
乳化剂:药用级十二烷基硫酸钠,2%;
去离子水:8% 。
其余同实施例1,组成复合淀粉膜的凝胶剂挤出膜与淀粉基挤出膜的单位面积重量比为1:16,制成的复合淀粉膜厚度为0.5mm。
实施例4
淀粉基挤出膜所用原料与重量比例如下:
淀粉:酯化木薯淀粉,85%;
抗结剂:药用级硬脂酸,1.2%;
糊化剂:去离子水,13.8% 。
凝胶剂挤出膜所用原料与重量比例如下:
凝胶剂:黄原胶,75%;
水分保持剂:药用级甘油,10%;
乳化剂:药用级十二烷基硫酸钠,4%;
去离子水:11% 。
其余同实施例1,组成复合淀粉膜的凝胶剂挤出膜与淀粉基挤出膜的单位面积重量比为1:16.2,制成的复合淀粉膜厚度为0.52mm。
实施例5
淀粉基挤出膜所用原料与重量比例如下:
淀粉:木薯淀粉,80%;
抗结剂:药用级硬脂酸,3.2%;
糊化剂:去离子水,16.8% 。
凝胶剂挤出膜所用原料与重量比例如下:
凝胶剂:交联木薯淀粉,85%;
水分保持剂:药用级山梨糖醇,8%;
乳化剂:药用级十二烷基硫酸钠,3%;
去离子水:4% 。
其余同实施例1,组成复合淀粉膜的凝胶剂挤出膜与淀粉基挤出膜的单位面积重量比为1:17,制成的复合淀粉膜厚度为0.47mm。
实施例6
淀粉基挤出膜所用原料与重量比例如下:
淀粉:玉米淀粉,85%;
抗结剂:药用级硬脂酸,1.2%;
糊化剂:去离子水,13.8%。
凝胶剂挤出膜所用原料与重量比例如下:
凝胶剂:卡拉胶,70%;
水分保持剂:药用级甘油,20%;
乳化剂:药用级十二烷基硫酸钠,2%;
去离子水:8% 。
其余同实施例1,组成复合淀粉膜的凝胶剂挤出膜与淀粉基挤出膜的单位面积重量比为1:13,制成的复合淀粉膜厚度为0.5mm。
对比实施例1
所使用的原料与重量比例如下:
凝胶剂:瓜尔胶,2%;
淀粉:玉米淀粉,80%;
水分保持剂:药用级甘油,1%;
抗结剂:药用级硬脂酸,0.2%;
乳化剂:药用级十二烷基硫酸钠,0.02%;
糊化剂:去离子水,16.78%。
将上述原料投入夹套釜中,再投入等重量的去离子水,升温至60℃,搅拌混合使充分溶胀和溶解,保温1-2h,形成胶液备用,依照通常制备软胶囊的方法制备软胶囊。
对比实施例2
淀粉基挤出膜所用原料与重量比例如下:
淀粉:玉米淀粉,85%;
抗结剂:药用级硬脂酸,1.2%;
糊化剂:去离子水,13.8% 。
凝胶剂糊液所用原料与重量比例如下:
凝胶剂:瓜尔胶,70%;
水分保持剂:药用级甘油,20%;
乳化剂:药用级十二烷基硫酸钠,2%;
去离子水:8% 。
双螺杆挤出机参数如下:
在螺杆的转动速度为350转/分钟的条件下挤出,其中各滑块设定的温度为:
滑块1: 25℃
滑块2-3: 110℃
滑块4-6: 145℃
滑块7-9: 165℃
滑块10-12: 160℃
喷嘴: 160℃
单螺杆挤出机的参数如下:
螺杆的转动速度为350转/分钟的,设定的温度为150℃
操作步骤如下:
(a)将淀粉和抗结剂放入高速混合机下以1500-2000rpm的转速,60℃下混合2min后搅拌混合,再将糊化剂在搅拌下缓缓加入高速混合机中,继续混合5min得淀粉基预混物料;
(b)将淀粉基预混物料投入双螺杆挤出机,挤出造粒得到淀粉基粒料,再使用单螺杆挤出机把淀粉基粒料制成膜,得到淀粉基挤出膜;
(c)将凝胶剂、水分保持剂和乳化剂溶于去离子水制成凝胶剂糊液,将凝胶剂糊液涂在淀粉挤出膜需要包封的内侧制成复合淀粉膜。
淀粉基胶囊制备步骤为:将共混膜放入加有温控的旋转冲模中制备出淀粉基胶囊,模具温度60℃。
各取实施例1-6的复合淀粉膜,对膜的断裂伸长度、拉伸模量进行检测,结果见表1。
各取上述8个实施例制备的软胶囊,对软胶囊装量差异、进行检查,按如下检查方法,结果见表1。
装量差异:按中国药典2010年版二部附录ⅠE所述方法检查,装量差异限度为±10%。采用常规方法在相同条件下测定其拉伸模量及断裂伸长度。
根据以上实施例,表明本发明方案所生产的软胶囊性能优越,符合药典标准,与现有技术相比具有极大的进步性。
表1:不同制备方式制得软胶囊的性能参数
Claims (4)
1.一种淀粉基软胶囊的制备方法,其特征在于,包含以下步骤:
(a)复合淀粉膜的制备:由淀粉、抗结剂和糊化剂预混制成淀粉基预混物料,将淀粉基预混物料投入双螺杆挤出机挤出造粒得到淀粉基粒料,再使用单螺杆挤出机把淀粉基粒料制成淀粉基挤出膜;再将凝胶剂、水分保持剂和乳化剂溶于水制成凝胶剂糊液,经单螺杆挤出机制成凝胶剂挤出膜,将凝胶剂挤出膜复合在淀粉挤出膜上经共挤制成复合淀粉膜,膜的厚度为0.2-1mm,拉伸模量大于3MPa,断裂伸长率为80%-140%;
(b)淀粉基软胶囊的制备:将两张复合淀粉膜,经旋转冲模法制成淀粉基软胶囊,
其中,组成复合淀粉膜的凝胶剂挤出膜与淀粉基挤出膜单位面积的重量比为1:10-1:20;
其中,所述的淀粉基预混物料的组成为:
淀粉:占淀粉基预混物料重量的80%-85%;
抗结剂:占淀粉基预混物料重量的1.2%-3.2%;
糊化剂:占淀粉基预混物料重量的13.8%-16.8%;
所述凝胶剂糊液的组成为:
凝胶剂:占凝胶剂糊液重量的70%-85%;
水分保持剂:占凝胶剂糊液重量的8%-20%;
乳化剂:占凝胶剂糊液重量的2%-4%;
其余为去离子水;
所述淀粉为各种天然来源的淀粉,或经物理、化学手段改性的淀粉;所述抗结剂为药用级硬脂酸或脂肪酸甘油酯;所述糊化剂为去离子水;所述凝胶剂选自支链淀粉、结冷胶、卡拉胶、黄原胶、瓜尔胶或各种植物胶的一种或多种组合;所述水分保持剂为药用级甘油或药用级山梨糖醇;所述乳化剂为药用级十二烷基硫酸的碱金属盐或十二烷基磺酸的碱金属盐。
2.根据权利要求1所述的制备方法,其特征在于,步骤(a)中,所述双螺杆挤出机参数为:物料温度在25-170℃之间,螺杆转速60-400转/分钟;所述单螺杆挤出参数为:物料温度在25-170℃之间,螺杆转速60-400转/分钟。
3.根据权利要求2所述的制备方法,其特征在于,所述单螺杆挤出参数为:物料温度在25-110℃之间,螺杆转速60-400转/分钟。
4.根据权利要求1所述的制备方法,其特征在于,将凝胶剂挤出膜复合在淀粉基挤出膜上的方法,将淀粉基挤出膜置于多层共挤机的下层辊筒,凝胶剂挤出膜置于上层辊筒,通过共挤模头挤出成复合淀粉膜。
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US6340473B1 (en) * | 1999-07-07 | 2002-01-22 | R.P. Scherer Technologies, Inc. | Film forming compositions comprising modified starches and iota-carrageenan and methods for manufacturing soft capsules using same |
ATE297433T1 (de) * | 1999-07-22 | 2005-06-15 | Warner Lambert Co | Filmbildende zusammensetzungen aus pullulan |
EP1103254B1 (de) * | 1999-11-19 | 2005-03-23 | Swiss Caps Rechte und Lizenzen AG | Verfahren zum Herstellen eines Stärke enthaltenden Formkörpers, homogenisierte Stärke enthaltende Masse und Vorrichtung zum Herstellen einer Weichkapsel |
US20050100640A1 (en) * | 2002-02-11 | 2005-05-12 | Pearce Tony M. | Microcapsule edibles |
DE50308456D1 (de) * | 2003-01-08 | 2007-12-06 | Swiss Caps Rechte & Lizenzen | Formkörper bestehend aus gelatinfreiem Material und gefüllt mit einer flüssigen Füllmasse |
US20050019294A1 (en) * | 2003-04-14 | 2005-01-27 | Fmc Corporation | Homogeneous, thermoreversible alginate films and soft capsules made therefrom |
US8231896B2 (en) * | 2004-11-08 | 2012-07-31 | R.P. Scherer Technologies, Llc | Non-gelatin soft capsule system |
CN1333006C (zh) * | 2005-04-07 | 2007-08-22 | 天津大学 | 淀粉组合物植物胶囊及制备方法 |
US8574624B2 (en) * | 2006-11-17 | 2013-11-05 | Corn Products Development, Inc. | Highly inhibited starch fillers for films and capsules |
CH700543A2 (de) * | 2009-03-03 | 2010-09-15 | Innogel Ag | Film auf Basis von Stärke. |
US8992971B2 (en) * | 2011-04-20 | 2015-03-31 | Suheung Capsule Co., Ltd. | Non-animal soft capsule shell composition having improved disintegration and shell hardness |
WO2013055668A1 (en) * | 2011-10-12 | 2013-04-18 | Dow Global Technologies Llc | Injection-molded dosage form |
-
2013
- 2013-10-26 CN CN201310510572.XA patent/CN103550065B/zh active Active
-
2014
- 2014-10-21 US US14/519,326 patent/US20150119470A1/en not_active Abandoned
- 2014-10-24 EP EP20140190242 patent/EP2865373A1/en active Pending
Also Published As
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EP2865373A1 (en) | 2015-04-29 |
CN103550065A (zh) | 2014-02-05 |
US20150119470A1 (en) | 2015-04-30 |
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