CN114795998B - 一种西红花苷双层包裹微囊的制备方法 - Google Patents
一种西红花苷双层包裹微囊的制备方法 Download PDFInfo
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- CN114795998B CN114795998B CN202210620872.2A CN202210620872A CN114795998B CN 114795998 B CN114795998 B CN 114795998B CN 202210620872 A CN202210620872 A CN 202210620872A CN 114795998 B CN114795998 B CN 114795998B
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- Prior art keywords
- saffron
- crocin
- microcapsule
- water phase
- water
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- 244000124209 Crocus sativus Species 0.000 title claims abstract description 37
- 235000015655 Crocus sativus Nutrition 0.000 title claims abstract description 37
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- 239000004248 saffron Substances 0.000 title claims abstract description 37
- 229930182478 glucoside Natural products 0.000 title claims abstract description 18
- 150000008131 glucosides Chemical class 0.000 title claims abstract description 18
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 52
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- 229910052751 metal Inorganic materials 0.000 claims abstract description 22
- 239000002184 metal Substances 0.000 claims abstract description 22
- 150000002338 glycosides Chemical class 0.000 claims abstract description 21
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- SEBIKDIMAPSUBY-JAUCNNNOSA-N Crocin Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C(=O)OC1OC(COC2OC(CO)C(O)C(O)C2O)C(O)C(O)C1O)C=CC=C(/C)C(=O)OC3OC(COC4OC(CO)C(O)C(O)C4O)C(O)C(O)C3O SEBIKDIMAPSUBY-JAUCNNNOSA-N 0.000 claims description 57
- SEBIKDIMAPSUBY-ARYZWOCPSA-N Crocin Chemical compound C([C@H]1O[C@H]([C@@H]([C@@H](O)[C@@H]1O)O)OC(=O)C(C)=CC=CC(C)=C\C=C\C=C(/C)\C=C\C=C(C)C(=O)O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O)O1)O)O[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O SEBIKDIMAPSUBY-ARYZWOCPSA-N 0.000 claims description 52
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- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 8
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- SGVYKUFIHHTIFL-UHFFFAOYSA-N Isobutylhexyl Natural products CCCCCCCC(C)C SGVYKUFIHHTIFL-UHFFFAOYSA-N 0.000 claims description 4
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- 239000000539 dimer Substances 0.000 claims description 4
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Abstract
本发明涉及一种西红花苷双层包裹微囊的制备方法，其特征在于采用以下步骤：A、按质量比称取西红花苷、金属螯合剂、银耳多糖、辅色剂、乳化剂、高分子聚合物、油脂，余量为水；B、将西红花苷、金属螯合剂、银耳多糖、辅色剂混合后加入到水中，搅拌均匀用作水相；C、将乳化剂、高分子聚合物、油脂混合后搅拌均匀用作油相；D、将水相与油相加入高压均质机进行均质，均质完成得西红花苷单层包裹微乳；E、制备外水相；F、将西红花苷单层包裹微乳和外水相，通过SPG膜乳化法将西红花苷单层包裹微乳加入到外水相中，得微囊悬浊液；G、将微囊悬浊液进行喷雾干燥，得西红花苷双层包裹微囊。本发明产物具有西红花苷不易褪色、稳定性好的优点。
Description
技术领域
本发明涉及微囊缓释技术领域，特别涉及一种西红花苷双层包裹微囊的制备方法。
背景技术
西红花苷是自然界唯一存在的水溶性类胡萝卜素类化合物，广泛存在于西红花中，又称为西红花素或藏红花素。目前主要作为天然的着色剂在食品、染料、化妆品行业中应用。西红花苷是一系列由西红花酸和不同糖结合成的酯苷，主要包括西红花苷Ⅰ、西红花苷Ⅱ、西红花苷Ⅲ、西红花苷Ⅳ等，其中西红花苷Ⅰ含量最高，约占70%~80%。西红花苷易溶于水成透明黄色溶液，可溶于乙醇和丙二酯，不溶于油脂。目前行业中，西红花苷常常直接被添加到产品中，但是西红花苷的稳定性较差，在加工和存储过程中暴露于热、氧气、光等环境，会产生失活、褪色的问题。因此如何保持西红花苷的稳定性成为研究重点。目前已知可使用两种方式增加其稳定性：其一，可以通过有效的提取富集方式来提高西红花苷稳定性，西红花苷的纯度越高，内部杂质含量越低，其稳定性越好。其二，通过与大分子物质的交联包埋形成复合物，降低在存储过程中的氧化分解，避免褪色。
现有技术中关于西红花苷的提取方法较多，如中国专利文献CN113144057A公开了一种西红花提取物及其制备方法和其应用，可高效提取西红花苷-I、西红花苷-Ⅱ和苦番红花素。但是对于西红花苷的后期包埋处理以避免氧化分解的相关研究较少。虽然有类胡萝卜素后期包埋制备方法的相关专利报道，如中国专利文献CN110772497A公开一种良好稳定的类胡萝卜素的微囊化方法，经拌装置搅拌、震荡和超声破碎，喷雾干燥后，制得类胡萝卜素微囊颗粒。但是其他类胡萝卜素类化合物都为油溶性的，而西红花苷则是水溶性的，现有的包埋类胡萝卜素的方式不适用于西红花苷，采用现有技术包埋西红花苷会存在包封率低，稳定时间短等技术问题。
发明内容
本发明要解决的技术问题是提供一种西红花苷双层包裹微囊的制备方法，该方法包封率高，且制备的西红花苷双层微囊具有不易褪色、稳定性好的优点。
为解决上述技术问题，本发明采用以下技术方案：一种西红花苷双层包裹微囊的制备方法，其特征在于采用以下步骤：
A、按以下质量百分比称取10~40%的西红花苷、0.1~1%的金属螯合剂、0.1~1%的银耳多糖、0.1~1%辅色剂，2~10%的乳化剂，2~5%高分子聚合物，2~15%油脂，余量为水；所述金属螯合剂为EDTA 二钠或硫酸镁，所述辅色剂为抗坏血酸、茶多酚、谷胱甘肽中的一种或它们的混合物；所述乳化剂为Span系列乳化剂；所述高分子聚合物为氢化（苯乙烯/甲基苯乙烯/茚）共聚物、二异硬脂酰基聚甘油-3二聚亚油酸酯、糊精异硬脂酸酯中的一种或它们的混合物；所述油脂为环状硅油、异十二烷、异十六烷中的一种或它们的混合物；
B、将步骤A称取的西红花苷、金属螯合剂、银耳多糖、辅色剂混合后加入到步骤A称取的水中，搅拌均匀用作水相；
C、将步骤A称取的乳化剂、高分子聚合物、油脂混合后搅拌均匀用作油相；
D、将步骤B所得水相与步骤C所得油相加入高压均质机进行均质，均质完成得西红花苷单层包裹微乳；
E、按质量比1:1:2~10:1:100称取水溶性大豆多糖、辛烯基琥珀酸淀粉钠和水，混合搅拌均匀后作为外水相；
F、按质量比1:1~1:3称取步骤D所得西红花苷单层包裹微乳和步骤E所得外水相，通过SPG膜乳化法将西红花苷单层包裹微乳加入到外水相中，得微囊悬浊液；
G、将步骤F所得微囊悬浊液进入喷雾干燥设备的喷枪中，设置进风温度90~130℃，出风温度40~60℃，进料流速5~20mL /min，进行喷雾干燥，得西红花苷双层包裹微囊。
本发明所述西红花苷购于上海哈灵生物科技有限公司。
本发明采用在包裹西红花苷的同时添加了金属螯合剂和辅色剂，所述金属螯合剂中含有Na+或Mg+，由于Na+或Mg+与西红花苷可以形成Na+或 Mg+—西红花苷复合物，然后再与大分子银耳多糖相互作用，能够很好地抑制西红花苷与水或其他物质发生作用，有效减缓西红花苷的化学降解。所述辅色剂可避免西红花苷被氧化分解成西红花酸，提高其稳定性。所以本发明在制备西红花苷双层微囊时加入金属螯合剂、银耳多糖、辅色剂可有效避免西红花苷的降解、褪色问题。
本发明在制备西红花苷的单层包裹微乳液选用高分子聚合物可在西红花苷外形成一层致密的高分子膜，包裹住西红花苷的同时由于其基团疏水，可有效避免后期西红花苷双层微囊加入水溶液后水分子进入微囊内部。但是高分子聚合物成膜后较脆，在形成微囊时容易发生断裂形成孔洞，导致较大孔隙，因而进行双层包裹，可有效地填充了微囊表面的孔隙。
本发明所述辛烯基琥珀酸淀粉钠具有良好的双亲性，其中的疏水基团—辛烯基可使其可快速地附着在西红花苷单层包裹微乳液上。同时辛烯基琥珀酸淀粉钠的亲水基团带负电荷，可与水溶性大豆多糖上的正电荷相结合。辛烯基琥珀酸淀粉钠和水溶性大豆多糖可共同构成第二层包裹壁材，且组合交联比单一组分制成壁材更加致密柔韧，不易破坏。
本发明所述SPG膜乳化法采用Ise Chemical Co.的SPG 膜乳化装置进行。膜乳化法是将均质乳化得到的W1/O初乳液滴在氮气的压力下通过SPG膜压入到外水相形成W1/O/W2双层乳液。采用SPG膜乳化法得到的乳液液滴粒径均一可控。
本发明通过喷雾干燥法可快速挥发水分和油分，制成双层包裹微囊。该西红花苷双层微囊呈固体粉末状态，便于长久保存，稳定性佳，且分散性好，便于加入化妆品中。
本发明中的西红花苷首先溶于水中，在进行第一层包裹时位于内相，且在进行第二次包裹时由于有第一层包裹阻隔，西红花苷不易释放，故包封率高，可达93.05%。
为证实本发明制备的西红花苷双层微囊具有不易褪色、稳定性好的优点，本发明进行了如下稳定性试验。
实施例1-3作为样品1-3；只经过单层包裹的西红花苷作为样品4；未进行包裹的西红花苷作为样品5。包裹时未添加金属螯合剂的西红花苷双层微囊作为样品6。包裹时未添加银耳多糖的西红花苷双层微囊作为样品7。包裹时未添加辅色剂的西红花苷双层微囊作为样品8。包裹时未添加金属螯合剂、银耳多糖、辅色剂的西红花苷双层微囊作为样品9。
将样品1-9分别配制成西红花苷质量含量为1%的水溶液，然后放置于5 ℃、25 ℃、45 ℃及光照条件下进行稳定性实验，并于2周、4周、8周和12周观察样品的颜色。稳定性测试结果见表1。
表1为稳定性测试结果
备注：0——表示无褪色； +——轻微褪色； ++——较严重褪色； +++——严重褪色。
从测试情况看，本发明制备的双层包裹微囊在经过三个月的稳定性实验，所有实施例均无变色的异常情况。而其他西红花苷样品均发生了不同程度的变色问题。说明西红花苷双层包裹微囊具有保护西红花苷不易褪色、稳定性好的优点。
具体实施方式
实施例1：一种西红花苷双层包裹微囊的制备方法，采用以下步骤：
A、按以下质量百分比称取10%的西红花苷、0.1%的金属螯合剂、0.1%的银耳多糖、0.1%辅色剂，2%的乳化剂，2%高分子聚合物，2%油脂，余量为水；所述金属螯合剂为EDTA 二钠，所述辅色剂为抗坏血酸；所述乳化剂为Span系列乳化剂；所述高分子聚合物为氢化（苯乙烯/甲基苯乙烯/茚）共聚物；所述油脂为环状硅油、异十二烷的混合物；
B、将步骤A称取的西红花苷、金属螯合剂、银耳多糖、辅色剂混合后加入到步骤A称取的水中，搅拌均匀用作水相；
C、将步骤A称取的乳化剂、高分子聚合物、油脂混合后搅拌均匀用作油相；
D、将步骤B所得水相与步骤C所得油相加入高压均质机进行均质，均质完成得西红花苷单层包裹微乳；
E、按质量比1:1:2称取水溶性大豆多糖、辛烯基琥珀酸淀粉钠和水，混合搅拌均匀后作为外水相；
F、按质量比1：1称取步骤D所得西红花苷单层包裹微乳和步骤E所得外水相，通过SPG膜乳化法将西红花苷单层包裹微乳加入到外水相中，得微囊悬浊液；
G、将步骤F所得微囊悬浊液进入喷雾干燥设备的喷枪中，设置进风温度90℃，出风温度40℃，进料流速5mL /min，进行喷雾干燥，得西红花苷双层包裹微囊。
实施例2：一种西红花苷双层包裹微囊的制备方法，采用以下步骤：
A、按以下质量百分比称取40%的西红花苷、1%的金属螯合剂、1%的银耳多糖、1%辅色剂， 10%的乳化剂， 5%高分子聚合物，15%油脂，余量为水；所述金属螯合剂为硫酸镁，所述辅色剂为茶多酚；所述乳化剂为Span系列乳化剂；所述高分子聚合物为二异硬脂酰基聚甘油-3二聚亚油酸酯；所述油脂为异十六烷；
B、将步骤A称取的西红花苷、金属螯合剂、银耳多糖、辅色剂混合后加入到步骤A称取的水中，搅拌均匀用作水相；
C、将步骤A称取的乳化剂、高分子聚合物、油脂混合后搅拌均匀用作油相；
D、将步骤B所得水相与步骤C所得油相加入高压均质机进行均质，均质完成得西红花苷单层包裹微乳；
E、按质量比10:1:100称取水溶性大豆多糖、辛烯基琥珀酸淀粉钠和水，混合搅拌均匀后作为外水相；
F、按质量比1：3称取步骤D所得西红花苷单层包裹微乳和步骤E所得外水相，通过SPG膜乳化法将西红花苷单层包裹微乳加入到外水相中，得微囊悬浊液；
G、将步骤F所得微囊悬浊液进入喷雾干燥设备的喷枪中，设置进风温度130℃，出风温度60℃，进料流速20mL /min，进行喷雾干燥，得西红花苷双层包裹微囊。
实施例3：一种西红花苷双层包裹微囊的制备方法，采用以下步骤：
A、按以下质量百分比称取25%的西红花苷、0.5%的金属螯合剂、0.5%的银耳多糖、0.5%辅色剂，6%的乳化剂，3%高分子聚合物，10%油脂，余量为水；所述金属螯合剂为EDTA 二钠，所述辅色剂为抗坏血酸、茶多酚、谷胱甘肽中的混合物；所述乳化剂为Span系列乳化剂；所述高分子聚合物为氢化（苯乙烯/甲基苯乙烯/茚）共聚物、二异硬脂酰基聚甘油-3二聚亚油酸酯、糊精异硬脂酸酯中的混合物；所述油脂为环状硅油、异十二烷、异十六烷中的混合物；
B、将步骤A称取的西红花苷、金属螯合剂、银耳多糖、辅色剂混合后加入到步骤A称取的水中，搅拌均匀用作水相；
C、将步骤A称取的乳化剂、高分子聚合物、油脂混合后搅拌均匀用作油相；
D、将步骤B所得水相与步骤C所得油相加入高压均质机进行均质，均质完成得西红花苷单层包裹微乳；
E、按质量比5:1:50称取水溶性大豆多糖、辛烯基琥珀酸淀粉钠和水，混合搅拌均匀后作为外水相；
F、按质量比1：2称取步骤D所得西红花苷单层包裹微乳和步骤E所得外水相，通过SPG膜乳化法将西红花苷单层包裹微乳加入到外水相中，得微囊悬浊液；
G、将步骤F所得微囊悬浊液进入喷雾干燥设备的喷枪中，设置进风温度120℃，出风温度50℃，进料流速12mL /min，进行喷雾干燥，得西红花苷双层包裹微囊。
Claims (1)
1.一种西红花苷双层包裹微囊的制备方法，其特征在于采用以下步骤：
A、按以下质量百分比称取10~40%的西红花苷、0.1~1%的金属螯合剂、0.1~1%的银耳多糖、0.1~1%辅色剂，2~10%的乳化剂，2~5%高分子聚合物，2~15%油脂，余量为水；所述金属螯合剂为EDTA 二钠或硫酸镁，所述辅色剂为抗坏血酸、茶多酚、谷胱甘肽中的一种或它们的混合物；所述乳化剂为Span系列乳化剂；所述高分子聚合物为氢化（苯乙烯/甲基苯乙烯/茚）共聚物、二异硬脂酰基聚甘油-3二聚亚油酸酯、糊精异硬脂酸酯中的一种或它们的混合物；所述油脂为环状硅油、异十二烷、异十六烷中的一种或它们的混合物；
B、将步骤A称取的西红花苷、金属螯合剂、银耳多糖、辅色剂混合后加入到步骤A称取的水中，搅拌均匀用作水相；
C、将步骤A称取的乳化剂、高分子聚合物、油脂混合后搅拌均匀用作油相；
D、将步骤B所得水相与步骤C所得油相加入高压均质机进行均质，均质完成得西红花苷单层包裹微乳；
E、按质量比1:1:2~10:1:100称取水溶性大豆多糖、辛烯基琥珀酸淀粉钠和水，混合搅拌均匀后作为外水相；
F、按质量比1:1~1:3称取步骤D所得西红花苷单层包裹微乳和步骤E所得外水相，通过SPG膜乳化法将西红花苷单层包裹微乳加入到外水相中，得微囊悬浊液；
G、将步骤F所得微囊悬浊液进入喷雾干燥设备的喷枪中，设置进风温度90~130℃，出风温度40~60℃，进料流速5~20mL /min，进行喷雾干燥，得西红花苷双层包裹微囊。
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