CN108652001B - 一种矢车菊素-3-葡萄糖苷复乳的制备方法 - Google Patents
一种矢车菊素-3-葡萄糖苷复乳的制备方法 Download PDFInfo
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Abstract
本发明公开了一种矢车菊素‑3‑葡萄糖苷复乳的制备方法，涉及营养保健领域。利用二步法制备复乳，初乳搅拌速率15500rpm；复乳搅拌速率7000rpm；内水相为pH＝2的柠檬酸溶液，其中含0.2％(w/w)黄原胶、0.1％NaCl(w/w)、浓度为1500ppm的矢车菊素‑3‑葡萄糖苷；油相为葵花籽油；外水相为蒸馏水，含有0.2％(w/w)黄原胶；亲油性乳化剂为聚甘油蓖麻醇酯，在油相中的含量为16％(w/w)；亲水性乳化剂为Span‑80/Tween80复配，HLB值为10，在外水相中的含量为10％(w/w)；内水相：油相：外水相＝15：35：50(w/w/w)。制得矢车菊素‑3‑葡萄糖苷复乳，包封率高，稳定性高。
Description
技术领域
本发明涉及营养保健领域，具体涉及花色苷复乳制备方法。
背景技术
矢车菊素-3-葡萄糖苷(C-3-G)是一种水溶性植物色素。具有有抗氧化、抗癌、改善肝功能、抗心血管疾病、抗炎、保护视力等多种生理作用。但其稳定性差，生物利用度低。
微囊可将活性物质包埋在内，提高活性物质的生物利用度。其中，复乳是一种两面三相的结构，有油包水包油(o/w/o)型和水包油包水(w/o/w)型。其中w/o/w型可将小分子水溶性物质包埋在内水相。复乳独特的结构赋予其保护、隔离、缓释、靶向释放等优良的性能。
目前已经有少量关于花色苷微囊方面的报道，已有报道表明微囊可促进花色苷在小肠部位的释放。但是，目前研究制得的花色苷微囊包封率都较低，粒径大，稳定性差，未创造花色苷所需的酸性环境，并且包裹的都是花色苷复合物。本发明内水相以柠檬酸创造pH＝2的酸性环境，以聚甘油蓖麻醇酯为油相乳化剂，Span-80/Tween80复配为亲水性乳化剂，黄原胶为稳定剂，用二步法制备高包封率，高稳定性的C-3-G复乳，以期促进花色苷类物质的广泛应用。
发明内容
本发明一种矢车菊素-3-葡萄糖苷复乳的制备方法，按照下述步骤进行：
(1)pH＝2柠檬酸溶液的配制；
(2)内水相的配制：将黄原胶0.4％(w/w)，NaCl 0.2％(w/w)溶于pH＝2的柠檬酸溶液中， 1000rpm磁力搅拌过夜；
(3)外水相的配制：外水相中亲水乳化剂为司班80/吐温80(Span-80/Tween80)复配，亲水亲油平衡值(HLB)为10，即Span-80含量为4.67％(w/w)，Tween80含量为5.33％(w/w)，总含量为10％(w/w)，黄原胶含量为0.2％(w/w)。按比例称取Span-80、Tween80、黄原胶于蒸馏水中，1000rpm磁力搅拌过夜；
(4)油相的配制：油相为葵花籽油，其中亲油性乳化剂为聚甘油蓖麻醇酯(PGPR)，含量为16％(w/w)。按比例称取PGPR于葵花籽油中，1000rpm磁力搅拌过夜；
(5)称取花色苷粉末，用pH＝2的柠檬酸溶液溶解，花色苷的浓度为3000ppm，将配置好的花色苷溶液按1:1(w/w)加入(2)所制得内水相中，避光、1000rpm磁力搅拌2h；
(6)将内水相和油相按3：7(w/w)称取，用高速分散仪15500rpm搅拌5min，制备初乳，过程中注意闭光；
(7)将第(6)步所制得初乳和外水相按1:1(w/w)称取，用高速分散仪7000rpm搅拌8min，制备复乳，过程中注意闭光。
本方法制得的C-3-G复乳，载药量为1500ppm，包封率为98.08％，3000rpm离心15min 乳层保留率为80.4％，稳定性好。
附图说明
图1为制备复乳的显微图片(10*100)。
具体实施方式
实施例1
(1)pH＝2柠檬酸溶液的制备：称取3.84g柠檬酸用100ML蒸馏水溶解，用pH计测其pH 值，用柠檬酸溶液和NaOH溶液微调，直到pH＝2；
(2)内水相的制备：称取黄原胶、NaCl溶于pH＝2柠檬酸溶液中，其中黄原胶含量为0.4％ (w/w)，NaCl含量为0.2％(w/w)，1000rpm磁力搅拌过夜；
(3)外水相的制备：按比例称取Span-80、Tween80、黄原胶溶于蒸馏水中，其中Span-80 含量为4.67％(w/w)，Tween80含量为5.33％(w/w)，黄原胶的含量为0.2％(w/w)，1000rpm 磁力搅拌过夜；
(4)油相的制备：按比例争取PGPR和葵花子油，其中PGPR含量为16％(w/w)，1000rpm 磁力搅拌过夜；
(5)称取C-3-G粉末，用pH＝2的柠檬酸溶液溶解，浓度为3000ppm，再将配置好的C-3-G 溶液和步骤(2)所得的内水相1:1(w/w)混合，避光，1000rpm磁力搅拌2h；
(6)初乳的制备：按3:7(w/w)称取步骤(5)所得的内水相和步骤(4)所得的油相，避光，用高速分散仪15500rpm搅拌5min，制得初乳；
(7)复乳的制备；按1:1(w/w)称取步骤(6)所得初乳和步骤(3)所得外水相，避光，用高速分散仪7000rpm搅拌8min，制得复乳。
本方法制得的C-3-G复乳，载药量为1500ppm，包封率为98.08％，粒径为688nm，电位为-27.61mV，3000rpm离心15min乳层保留率为85.17％，稳定性好。
对比例1
Mónica Escobar Blanco等用二步法制备花色苷复乳，第一步将花色苷溶液缓慢滴入含有乳化剂的油相中，油相乳化剂为PGPR和Panodan，其中PGPR含量为6％(w/w)，Panodan 含量为4％，内水相和油相的比例为1:1(w/w)，7600rpm搅拌15min，制备初乳。第二步将初乳按照1:1(w/w)加入含有12.5％分离乳清蛋白溶液中，600rpm搅拌10min，制得花色苷复乳，该复乳体系未创造酸性环境，粒径为4.74μm，粒径较大。本对比例为文献EscobarBlanco M,Quezada Gallo J A,Estrada Arias K S,et al.Colorimetry Technique as aTool for Determining Release Kinetics and Mass Transfer Parameters ofAnthocyanins Encapsulated in W1/O/W2 Double Emulsions[J].InternationalJournal of Food Engineering,2016,12(7):615-624.中报道的方法！
对比例2
韩爱芝等在60℃条件下，将阿拉伯胶用pH值为3缓冲液溶解，再加入β-环糊精，待壁材完全溶解后冷却至室温，乳化均质后，经喷雾干燥制备花色苷微囊，得到微囊包封率为91.01％，平均粒径为9.16μm。本对比例为文献“韩爱芝,蒋卉,贾清华,等.响应面试验优化黑果枸杞花色苷微胶囊制备工艺及其稳定性分析[J].食品科学,2016,37(10):82-87.”中报道的方法。
Claims (1)
1.一种矢车菊素-3-葡萄糖苷复乳的制备方法，其特征在于按照下述步骤进行：
(1)pH＝2柠檬酸溶液的配制；
(2)内水相的配制：将黄原胶0.4％(w/w)，NaCl 0.2％(w/w)溶于pH＝2的柠檬酸溶液中，1000rpm磁力搅拌过夜；
(3)外水相的配制：外水相中亲水乳化剂为司班80/吐温80(Span-80/Tween80)复配，亲水亲油平衡值(HLB)为10，按比例称取Span-80、Tween80、黄原胶于蒸馏水中，1000rpm磁力搅拌过夜；
(4)油相的配制：油相为葵花籽油，其中亲油性乳化剂为聚甘油蓖麻醇酯(PGPR)，含量为16％(w/w)；按比例称取PGPR于葵花籽油中，1000rpm磁力搅拌过夜；
(5)称取花色苷粉末，用pH＝2的柠檬酸溶液溶解，花色苷的浓度为3000ppm，将配置好的花色苷溶液按1:1(w/w)加入(2)所制得内水相中，避光、1000rpm磁力搅拌2h；
(6)将内水相和油相按3：7(w/w)称取，用高速分散仪15500rpm搅拌5min，制备初乳，过程中注意闭光；
(7)将第(6)步所制得初乳和外水相按1:1(w/w)称取，用高速分散仪7000rpm搅拌8min，制备复乳；
步骤(3)中Span-80含量为4.67％(w/w)，Tween80含量为5.33％(w/w)，总含量为10％(w/w)，黄原胶含量为0.2％(w/w)。
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| EP2162009A1 (en) * | 2007-06-29 | 2010-03-17 | Nestec S.A. | Stable double emulsions |
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| CN102362858A (zh) * | 2011-11-07 | 2012-02-29 | 江南大学 | 一种搭载药物的微小粒径的w/o/w型多重乳状液的制备方法 |
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