CN115382502A - 甘草三萜苷硅酸盐蒙脱石络合物的制备方法、络合物及其应用 - Google Patents
甘草三萜苷硅酸盐蒙脱石络合物的制备方法、络合物及其应用 Download PDFInfo
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- CN115382502A CN115382502A CN202211005896.3A CN202211005896A CN115382502A CN 115382502 A CN115382502 A CN 115382502A CN 202211005896 A CN202211005896 A CN 202211005896A CN 115382502 A CN115382502 A CN 115382502A
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- Prior art keywords
- montmorillonite
- glycyrrhiza
- complex
- glycoside
- silicate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 title claims abstract description 108
- 229910052901 montmorillonite Inorganic materials 0.000 title claims abstract description 100
- 241000202807 Glycyrrhiza Species 0.000 title claims abstract description 37
- 229930182470 glycoside Natural products 0.000 title claims abstract description 34
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 title claims abstract description 21
- LTINPJMVDKPJJI-UHFFFAOYSA-N iodinated glycerol Chemical compound CC(I)C1OCC(CO)O1 LTINPJMVDKPJJI-UHFFFAOYSA-N 0.000 title claims abstract description 18
- XBZYWSMVVKYHQN-MYPRUECHSA-N (4as,6as,6br,8ar,9r,10s,12ar,12br,14bs)-10-hydroxy-2,2,6a,6b,9,12a-hexamethyl-9-[(sulfooxy)methyl]-1,2,3,4,4a,5,6,6a,6b,7,8,8a,9,10,11,12,12a,12b,13,14b-icosahydropicene-4a-carboxylic acid Chemical compound C1C[C@H](O)[C@@](C)(COS(O)(=O)=O)[C@@H]2CC[C@@]3(C)[C@]4(C)CC[C@@]5(C(O)=O)CCC(C)(C)C[C@H]5C4=CC[C@@H]3[C@]21C XBZYWSMVVKYHQN-MYPRUECHSA-N 0.000 title claims abstract description 14
- 150000002338 glycosides Chemical class 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- -1 glycyrrhiza triterpenoid glycoside Chemical class 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 41
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- 238000003756 stirring Methods 0.000 claims description 22
- 239000002002 slurry Substances 0.000 claims description 20
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 18
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- LPLVUJXQOOQHMX-QWBHMCJMSA-N glycyrrhizinic acid Chemical compound O([C@@H]1[C@@H](O)[C@H](O)[C@H](O[C@@H]1O[C@@H]1C([C@H]2[C@]([C@@H]3[C@@]([C@@]4(CC[C@@]5(C)CC[C@@](C)(C[C@H]5C4=CC3=O)C(O)=O)C)(C)CC2)(C)CC1)(C)C)C(O)=O)[C@@H]1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@H]1O LPLVUJXQOOQHMX-QWBHMCJMSA-N 0.000 claims description 15
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 14
- 239000011734 sodium Substances 0.000 claims description 14
- 229910052708 sodium Inorganic materials 0.000 claims description 14
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 12
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- JGSARLDLIJGVTE-MBNYWOFBSA-N Penicillin G Chemical compound N([C@H]1[C@H]2SC([C@@H](N2C1=O)C(O)=O)(C)C)C(=O)CC1=CC=CC=C1 JGSARLDLIJGVTE-MBNYWOFBSA-N 0.000 description 3
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/10—Organic substances
- A23K20/116—Heterocyclic compounds
- A23K20/121—Heterocyclic compounds containing oxygen or sulfur as hetero atom
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/20—Inorganic substances, e.g. oligoelements
- A23K20/28—Silicates, e.g. perlites, zeolites or bentonites
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- A—HUMAN NECESSITIES
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/70—Carbohydrates; Sugars; Derivatives thereof
- A61K31/7028—Compounds having saccharide radicals attached to non-saccharide compounds by glycosidic linkages
- A61K31/7034—Compounds having saccharide radicals attached to non-saccharide compounds by glycosidic linkages attached to a carbocyclic compound, e.g. phloridzin
- A61K31/704—Compounds having saccharide radicals attached to non-saccharide compounds by glycosidic linkages attached to a carbocyclic compound, e.g. phloridzin attached to a condensed carbocyclic ring system, e.g. sennosides, thiocolchicosides, escin, daunorubicin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/04—Antibacterial agents
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Abstract
本发明公开了一种甘草三萜苷硅酸盐蒙脱石络合物的制备方法、络合物及其应用,在酸性条件下,选用具有抗菌抗病毒功效的甘草三萜苷作为改性剂与蒙脱石络合,利用甘草三萜苷中的羧基与蒙脱石层边缘的羟基相互作用,既扩大了蒙脱石层间域,加强其对霉菌毒素等有害物的吸附能力,又能够发挥甘草三萜苷的抗菌抗病毒活性,从而达到一加一大于二的效果,在饲料替抗中有着广阔的运用前景。本发明所制备的络合物在理论作用机理上具有优秀的抗菌抗病毒活性,同时在应用中也展现出了明显的作用效果。本发明提供的络合物能够用于禽畜等动物的饲料中,发挥替代抗生素的作用。
Description
技术领域
本发明涉及蒙脱石络合物及其制备技术领域,尤其涉及一种甘草三萜苷硅酸盐蒙脱石络合物的制备方法、络合物及其应用。
背景技术
蒙脱石是一种片层间含有少量碱或碱土金属的2:1型层状硅酸盐矿物,每个层都是由两个硅氧(Si-O)四面体层中间夹着铝氧(Al-O-(OH))八面体层组成。近年来针对蒙脱石有机无机杂化材料的研究愈来愈多,这种材料通常是通过阳离子交换、表面吸附或接枝得到的,一般选用有机阳离子、阴离子、两性离子、非离子作为有机插层剂。经过有机改性的蒙脱石材料能够增加其层间域,相应地提高了其吸附能力,能够广泛用于病毒、有机污染物、重金属和染料的吸附。
中国专利CN1554474A一种阳-非离子有机膨润土废水处理材料的制备方法提供了一种制备阳、非离子型有机蒙脱石的方法,其步骤为将干燥、粉碎过20~100目筛的膨润土原土倒入一定配比的混合表面活性剂溶液中,在50~80℃水浴中搅拌2~24h,产物经过滤,用蒸馏水洗涤2次,滤干后,在60~90℃下烘干,再在105℃下活化30min~5h,经研磨,过100目筛,制得阳-非离子有机膨润土。该发明所制备的材料对水中有机污染物吸附能力显著增强,但工艺反应时间长且工艺繁琐。
目前国内外阳离子蒙脱石有机无机杂化材料研究较多,与其相比,阴离子蒙脱石有机无机杂化材料具有更出色的热稳定性。部分研究人员认为由于带负电的蒙脱石片层与带负电的有机阴离子头部之间存在静电排斥,使得有机阴离子无法插入蒙脱石的层间域中。然而也有一部分研究人员提出新的观点并通过实验证明,有机阴离子可以通过与蒙脱石层边缘的羟基相互作用或离子偶极相互作用进入蒙脱石的层间空间。酸性介质会促进氢离子交换,使得酸侵蚀蒙脱石各层的电荷位点,从而导致蒙脱石晶体部分溶解。蒙脱石被酸侵蚀能够帮助有机阴离子渗透到蒙脱石各层间。Zhang等在酸性介质中通过超声处理合成十二烷基硫酸钠和十八烷基碳酸钠的蒙脱石有机无机杂化材料,晶面间距分别增加到3.87nm和4.80nm。Yu等在酸性介质(pH=1)和强力搅拌下合成了十二烷基磺酸钠/钙基蒙脱石有机无机杂化材料,晶面间距增加到1.52nm。这些实验与理论为甘草三萜苷与蒙脱石络合提供了支撑。另有中国专利CN103109980A一种提高免疫力的中草药饲料添加剂、制备方法及饲料,公开的饲料组成成分以及重量数为:千屈菜、红背菜、山药、淫羊藿、焦神曲、鸡藤、葛根、升麻、芍药、建曲、大黄、厚朴、贯众、甘草、黄芩、忍冬藤、绞股蓝、茯苓、大豆异黄酮、大豆皂甙、附加成分,所述附加成分是维生素A、维生素B、维生素C、三氯化铬、黄元胶、木糖醇、甘露醇结晶,所述附加成分的各组成部分配比为0.2∶0.2∶0.5∶0.3∶1∶1∶1。该发明提供的饲料添加剂有一定免疫调节和抗菌效果,但是配方复杂,加工粗糙,作用效果不够稳定,无法真正替代抗生素。
研究显示,甘草三萜苷类化合物具有特定的抗菌和抗病毒活性。其中一些皂苷表现为有抗菌活性较强,一些皂苷表现为有抗病毒活性较强。而蒙脱石对消化道内的病毒、病菌、霉菌毒素、气体等有极强的吸附、固定、抑制作用,同时对微生物次级代谢物如芳香族化合物、氨、内毒素也有较好的吸附效果。在酸性条件下,利用甘草三萜苷中的羧基与蒙脱石层边缘的羟基相互作用,既扩大了蒙脱石层间域,加强其对霉菌毒素等有害物的吸附能力,又能够发挥甘草三萜苷的抗菌抗病毒活性,从而达到一加一大于二的效果,在饲料替抗中有着广阔的运用前景。
发明内容
发明目的:为了克服现有技术中存在的问题,本发明提出了一种甘草三萜苷硅酸盐蒙脱石络合物的制备方法、络合物及其应用,在抗菌抗病毒、预防动物疾病方面具有积极效果,可以作为安全高效的饲用抗生素替代产品在动物生产中应用。
技术方案:为了解决上述技术问题,本发明所采用的技术方案为:
一种甘草三萜苷硅酸盐蒙脱石络合物的制备方法,包括如下步骤:
1)提纯:将钙基蒙脱石充分分散在去离子水中,继续搅拌,静置沉降,去除底部沉淀,取上层悬浮液离心得提纯后的钙基蒙脱石;
2)钠化:取提纯后的钙基蒙脱石分散在去离子水中,添加其质量2-6%的碳酸钠,搅拌,离心;用去离子水洗去未反应的碳酸钠和交换出的钙离子得钠基蒙脱石;
3)超声处理;取钠基蒙脱石分散在去离子水中,温度控制在50-100℃,超声处理;同时机械搅拌得蒙脱石浆液;
4)合成:在蒙脱石浆液中加入甘草三萜苷;用HCl调节pH为1-5,搅拌、静置、冷却、离心,用温水洗;60-100℃干燥,研磨过200目筛得甘草三萜苷硅酸盐蒙脱石络合物。
更进一步的,步骤1)中钙基蒙脱石和去离子水的固液比为1:10~1:100,搅拌时间为1~8h。
更优选的,钙基蒙脱石:水固液比为1:20,搅拌时间为4h。
更进一步的,步骤2)中的钙基蒙脱石和去离子水的固液比为1:20~1:100,搅拌时间为1~8h;离心后水洗用量为钙基蒙脱石重量的60~200倍。
更优选的,钙基蒙脱石:水固液比为1:20,搅拌时间为3h。
更进一步的,步骤3)中的超声处理过程中,钠基蒙脱石和去离子水的固液比为1:20~1:200,超声处理温度为60℃,时间为1~6h。
更优选的,钠基蒙脱石:水固液比为1:20;超声处理时间为1~3h。。
更进一步的,步骤4)甘草三萜苷添加量为蒙脱石质量的5%~30%,HCl调酸pH在1~5;搅拌条件为温度40~120℃,时间2~12h;离心后温水洗涤用量为10~200倍钠基蒙脱石质量,干燥温度为80℃。更优选的,甘草三萜苷添加量为10%~60%,反应温度为60℃,时间6h。
更进一步的,步骤4)中甘草三萜苷为甘草酸、乌拉尔甘草皂苷A、B和甘草皂苷A3、B2、C2、D3、E2、F3、G2、H2、J2、K2中的一种或多种。
本发明还公开了上述制备方法制备的甘草三萜苷硅酸盐蒙脱石络合物。
本发明还公开了上述甘草三萜苷硅酸盐蒙脱石络合物的应用,具体用于饲料替抗中。
有益效果:
(1)本发明在酸性条件下,选用具有抗菌抗病毒功效的甘草三萜苷作为改性剂与蒙脱石络合,利用甘草三萜苷中的羧基与蒙脱石层边缘的羟基相互作用,既扩大了蒙脱石层间域,加强其对霉菌毒素等有害物的吸附能力,又能够发挥甘草三萜苷的抗菌抗病毒活性,从而达到一加一大于二的效果,在饲料替抗中有着广阔的运用前景。
(2)本发明工艺流程简单,原料来源易得,产品层间距高,热稳定性高。
具体实施方式
下面结合实施例对本发明作进一步的详细说明:
实施例1:
1)提纯:取100g钙基蒙脱石充分分散在2000g去离子水中,电动搅拌器1000r/min搅拌4h,室温静置沉降6h,去除底部沉淀,取上层悬浮液4500r/min离心10min,将所得下层沉淀物60℃干燥24h,粉碎过200目筛;
2)钠化:取50g提纯后的钙基蒙脱石分散在1000g去离子水中,电动搅拌器搅拌1h,添加2g碳酸钠,继续搅拌2h;离心,离心后的产物用5L去离子水洗去未反应的碳酸钠和交换出的钙离子;干燥粉碎过200目筛。
3)超声处理:取2g钠基蒙脱石分散在200g去离子水中,温度控制在60℃,超声处理5h;同时机械搅拌3h得蒙脱石浆液;
4)合成:在蒙脱石浆液中加入1g甘草酸铵;HCl调酸pH=3;60℃搅拌6h;恒温静置2h,冷却、离心,用400g温水洗;80℃干燥,研磨过200目筛得甘草三萜苷硅酸盐蒙脱石络合物。
实施例2:
其他实施方式与实施例1相同,不同之处在于步骤3)和4),具体如下:
3)超声处理;取50g钠基蒙脱石于1000g去离子水中,温度控制在60℃,超声分散,同时机械搅拌3h得到蒙脱石浆液;
4)合成:在浆液中加入20g甘草酸铵;HCl调酸pH=3;60℃搅拌6h;恒温静置2h,离心分离固液,用2000g温水洗涤两次;80℃干燥,研磨过200目筛。
实施例3:
其他实施方式与实施例1相同,不同之处在于步骤3)和4),具体如下:
3)超声处理;取50g钠基蒙脱石分散在1000g去离子水中,温度控制在60℃,超声分散,同时机械搅拌1h得到蒙脱石浆液;
4)合成:在浆液中加入5g甘草酸铵;HCl调酸pH=3;60℃搅拌6h;恒温静置2h,离心分离固液,用2000g温水洗涤两次;80℃干燥,研磨过200目筛。
实施例4:
其他实施方式与实施例1相同,不同之处在于步骤3)和4),具体如下:
3)超声处理;取50g钠基蒙脱石分散在1000g去离子水中,温度控制在60℃,超声分散,同时机械搅拌1h得到蒙脱石浆液;
4)合成:在浆液中加入30g甘草酸铵;HCl调酸pH=3;60℃搅拌6h;恒温静置2h,离心分离固液,用2000g温水洗涤两次;80℃干燥,研磨过200目筛。
实施例5:
其他实施方式与实施例1相同,不同之处在于步骤3)和4),具体如下:
3)超声处理;取50g钠基蒙脱石分散在1000g去离子水中,温度控制在60℃,超声分散,同时机械搅拌1h得到蒙脱石浆液;
4)合成:在浆液中加入20g甘草酸铵;HCl调酸pH=1;60℃搅拌6h;恒温静置2h,离心分离固液,用2000g温水洗涤两次;80℃干燥,研磨过200目筛。
实施例6:
其他实施方式与实施例1相同,不同之处在于步骤3)和4),具体如下:
3)超声处理;取50g钠基蒙脱石分散在1000g去离子水中,温度控制在60℃,超声分散,同时机械搅拌1h得到蒙脱石浆液;
4)合成:在浆液中加入20g甘草酸铵;HCl调酸pH=5;60℃搅拌6h;恒温静置2h,离心分离固液,用2000g温水洗涤两次;80℃干燥,研磨过200目筛。
实施例7:
其他实施方式与实施例1相同,不同之处在于步骤3)和4),具体如下:
3)超声处理;取50g钠基蒙脱石分散在1000g去离子水中,温度控制在60℃,超声分散,同时机械搅拌1h得到蒙脱石浆液;
4)合成:在浆液中加入20g甘草酸铵;HCl调酸pH=3;60℃搅拌2h;恒温静置2h,离心分离固液,用2000g温水洗涤两次;80℃干燥,研磨过200目筛。
实施例8:
其他实施方式与实施例1相同,不同之处在于步骤3)和4),具体如下:
3)超声处理;取50g钠基蒙脱石分散在1000g去离子水中,温度控制在60℃,超声分散,同时机械搅拌1h得到蒙脱石浆液;
4)合成:在浆液中加入20g甘草酸铵;HCl调酸pH=3;60℃搅拌12h;恒温静置2h,离心分离固液,用2000g温水洗涤两次;80℃干燥,研磨过200目筛。
对比例1:未进行改性处理的市售钙基蒙脱石
应用和分析:
(一)最优条件分析
对实施例1-8中制备的络合物进行负载量检测,测试方法与结果如下:
取合成离心后的上清液进行HPLC检测,测得未与蒙脱石络合的甘草酸铵含量,即可算出蒙脱石的负载量。
蒙脱石的负载量=络合的甘草酸铵质量/蒙脱石质量
=(甘草酸铵添加量-未络合的甘草酸铵质量)/蒙脱石质量
HPLC条件:
色谱柱:C18柱(4.6mm*250mm,5μm)
流动相:2%冰醋酸:乙腈=65:35
流速:1.0mL/min
检测波长:256nm
柱温30℃
进样量:20μL
表1实施例1-8制备的络合物负载量
添加剂性能测试:
对测得负载量结果较为优越的络合物实施例1、2、4、8以及对比例1进行性能检测,检测其耐酸性和耐温性,接测结果如表2所示:
耐酸性试验:验证饲料添加剂过胃酸的能力。在pH≤2,2-4小时检测其存留量。
耐温性实验:为了验证在饲料调质条件下存留率,耐温试验需要在80℃-125℃温度下,水浴5分钟。
表2实施例以及对比例1制备的添加剂性能
耐酸性 | 耐温性 | |
实施例1 | pH=1,无损失 | 耐温≤125℃ |
实施例2 | pH=1,无损失 | 耐温≤125℃ |
实施例4 | pH=1,无损失 | 耐温≤125℃ |
实施例8 | pH=1,无损失 | 耐温≤125℃ |
对比例1 | pH=1,无损失 | 耐温≤125℃ |
结合制备所需的原料、能量消耗,最终选择方案实施例1为最佳方案,进行大批量制备用于动物实验。
(二)饲料添加剂应用肉鸡投喂实验:
实验对象:选择生长条件、健康状况一致,1天龄的160只肉鸡,随机分为4组(空白对照组、阳性对照组、蒙脱石对照组,试验组),每组均为40只;连续喂养六周,空白对照组喂食常规日粮,阳性对照以青霉素为对照,添加量按照文献所用100g/t,蒙脱石对照组在日粮的基础上添加对比例1中未经改性的钙基蒙脱石,用量为60g/t;试验组在日粮的基础上添加本发明实施例1制备的甘草三萜苷硅酸盐蒙脱石络合物,用量为60g/t。
结果如表3所示。
表3肉鸡投喂实验结果
(三)饲料添加剂应用蛋鸡投喂实验:
实验对象:选择生长条件、健康状况一致,40周龄的160只蛋鸡,随机分为三组(空白对照组、阳性对照组、蒙脱石对照组、试验组),每组均为40只;连续喂养八周,空白对照组喂食常规日粮,阳性对照以青霉素为对照,添加量按照文献所用100g/t,蒙脱石对照组在日粮的基础上添加对比例1中未经改性的钙基蒙脱石,用量为60g/t;试验组在日粮的基础上添加本发明实施例1制备的甘草三萜苷硅酸盐蒙脱石络合物,用量为60g/t。
结果如表4所示。
表4蛋鸡投喂实验结果
从以上实验结果可以看出,无论是肉鸡还是蛋鸡,试验组的日粮添加了本发明实施例1制备的络合物投喂效果明显好于空白对照组、蒙脱石对照组,阳性对照组,用量少且吸收好,说明本发明中制备的甘草三萜苷硅酸盐蒙脱石络合物在饲料替抗中具有良好的作用。
最后所应当说明的是,以上实施例仅用以说明本发明的技术方案而非对本发明保护范围的限制,尽管参照较佳实施例对本发明作了详细说明,本领域的普通技术人员应当理解,可以对本发明的技术方案进行修改或者等同替换,而不脱离本发明技术方案的实质和范围。
Claims (8)
1.一种甘草三萜苷硅酸盐蒙脱石络合物的制备方法,其特征在于包括如下步骤:
1)提纯:将钙基蒙脱石充分分散在去离子水中,继续搅拌,静置沉降,去除底部沉淀,取上层悬浮液离心得提纯后的钙基蒙脱石;
2)钠化:取提纯后的钙基蒙脱石分散在去离子水中,添加蒙脱石质量2-6%的碳酸钠,搅拌,离心;用去离子水洗去未反应的碳酸钠和交换出的钙离子得钠基蒙脱石;
3)超声处理;取钠基蒙脱石分散在去离子水中,温度控制在50-100℃,超声处理;同时机械搅拌得蒙脱石浆液;
4)合成:在蒙脱石浆液中加入甘草三萜苷;用HCl调节pH为1-5,搅拌、静置、冷却、离心,用温水洗;60-100℃干燥,研磨过200目筛得甘草三萜苷硅酸盐蒙脱石络合物。
2.根据权利要求1所述的甘草三萜苷硅酸盐蒙脱石络合物的制备方法,其特征在于:步骤1)中钙基蒙脱石和去离子水的固液比为1:10~1:100,搅拌时间为1~8h。
3.根据权利要求1所述的甘草三萜苷硅酸盐蒙脱石络合物的制备方法,其特征在于:步骤2)中的钙基蒙脱石和去离子水的固液比为1:20~1:100,搅拌时间为1~8h;离心后水洗用量为钙基蒙脱石重量的60~200倍。
4.根据权利要求1所述的甘草三萜苷硅酸盐蒙脱石络合物的制备方法,其特征在于:步骤3)中的超声处理过程中,钠基蒙脱石和去离子水的固液比为1:20~1:200,超声处理温度为60℃,处理时间为1~6h。
5.根据权利要求1所述的甘草三萜苷硅酸盐蒙脱石络合物的制备方法,其特征在于:步骤4)中甘草三萜苷添加量为钠基蒙脱石质量的5%~30%,HCl调酸pH在1~5;搅拌条件为温度40~120℃,时间2~12h;离心后温水洗涤用量为10~200倍钠基蒙脱石质量,干燥温度为80℃。
6.根据权利要求1所述的甘草三萜苷硅酸盐蒙脱石络合物的制备方法,其特征在于:步骤4)中甘草三萜苷为甘草酸、乌拉尔甘草皂苷A、B和甘草皂苷A3、B2、C2、D3、E2、F3、G2、H2、J2、K2中的一种或多种。
7.一种权利要求1所述的制备方法制备的甘草三萜苷硅酸盐蒙脱石络合物。
8.一种权利要求1-7任一项所述的甘草三萜苷硅酸盐蒙脱石络合物的应用,其特征在于在饲料替抗中的应用。
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