CN113208017A - 一种酸梅汤及其制备方法 - Google Patents
一种酸梅汤及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种酸梅汤及其制备方法。所述酸梅汤的制备原料包括如下重量份数的原料：山楂果100‑150份、乌梅100‑150份、甘草10‑30份、陈皮30‑80份，桂花5‑15份，越橘30‑80份。本发明的酸梅汤制备原料引入越橘，越橘含有大量的原花青素，与酸梅汤中的其他组分共煮能最大限度的保留原花青素，尤其是原花青素中的EC、B2、C1聚合程度低的组分，使得花青素营养物质易于被人体吸收利用。
Description
技术领域
本发明属于天然饮料制备技术领域，具体涉及一种高原花青素含量的酸梅汤及其制备方法。
背景技术
酸梅汤是传统的消暑饮料，制作原料主要有乌梅、山楂、陈皮、桂花、甘草、冰糖等材料。酸梅汤作为传统饮料，清爽爽口，时常喝一杯酸梅汤不仅可以去油解腻，还可以健脾开胃，提神醒脑。
酸梅汤中的营养物质主要有原花青素、多酚、黄酮、果胶、矿物质、蛋白质、氨基酸、膳食纤维和多种微量元素。原花青素是一类能在酸性加热条件下生成花色素的缩合多酚类化合物，通常以黄烷-3-醇类为主要结构单元，最早于1960年由Weinges提出，泛指能够在热酸处理下生成花色素的物质，在当时得到了公认并沿用至今。研究发现，原花青素是由数量不同的儿茶素、表儿茶素、棓儿茶素、表棓儿茶素或没食子酸表儿茶素酯缩合而成的聚合体。不同来源的原花青素分子，单体组成以及聚合程度都有明显的差异。通常将聚合度为二-六聚体的原花青素称为低聚或寡聚原花青素(oligomeric proanthocyanidins，OPC)，它又可分为B、C、D、E、F等不同聚合度的聚合体。六聚体以上的称为高聚或多聚原花青素(polymeric proanthocyanidins，PPC)。根据组成和连接方式的不同，二聚体共有8种分子结构，它们分别被称为前花青素B1、B2……直到B8；同理，三聚体会有32种结构、四聚体会有128种结构、五聚体有512种。有研究表明只有聚合度小于3的原花青素易于通过肠道内皮细胞被机体吸收利用，而聚合度较大的原花青素因空间结构阻碍等因素不能直接被机体吸收，造成原花青素的大量损失。
Thompson研究发现，原花青素在酸性条件下加热可以被分解，黄烷醇单元之间的C-C键发生断裂，当体系中有亲核试剂如苄硫醇存在时，断裂反应之后原来的化学键的“下部”生成一个黄烷醇分子，而化学键的“上部”生成一个黄烷醇的苄硫醚衍生物。这种断裂衍生化反应可以在原花青素各结构单元之间随机发生，直到最后，原花青素聚合物分子中各单元间的C-C键全部断裂并生成相应的末端黄烷醇单体以及它们的苄硫醚衍生物。酸梅汤的制备过程中需要长时间熬煮，溶液呈酸性，因此原花青素的损失较大。
发明内容
本发明的目的在于提供一种高原花青素含量的酸梅汤及其制备方法。
一种酸梅汤，所述酸梅汤的制备原料包括如下重量份数的原料：山楂果100-150份、乌梅100-150份、甘草10-30份、陈皮30-80份，桂花5-15份，越橘30-80份。
所述酸梅汤中的原花青素以EC、B2、C1为主，聚合程度低。
所述原花青素的结构通式如图1所示；原花青素主要单体的结构如图2所示。
所述酸梅汤的制备方法，按照如下步骤进行：
(1)按照重量份数，取山楂果100-150份、乌梅100-150份、甘草10-30份、陈皮30-80份，桂花5-15份，越橘30-80份，清洗干净；
(2)取洗净的山楂果和乌梅，加入3-15倍重量份数的水，熬煮锅中煮开后再熬煮20-35min；
(3)加入甘草、陈皮和越橘继续熬煮20-30min，再加入桂花继续熬煮3-6min；
(4)降温至室温捞渣，剩余液体过滤后加入占滤液质量1-6％的糖，灌装杀菌制成。
所述糖为白砂糖、绵白糖或者红糖。
所述灌装杀菌为水浴杀菌，杀菌温度为95℃，杀菌时间30min。
所述酸梅汤的色泽为7580C-7600C。
所述酸梅汤的PH为3.0-4.0；折光为12.0-14.0。
本发明的有益效果：本发明的酸梅汤制备原料引入越橘，越橘含有大量的原花青素，与酸梅汤中的其他组分共煮能最大限度的保留原花青素，尤其是原花青素中的EC、B2、C1聚合程度低的组分，使得花青素营养物质易于被人体吸收利用。
附图说明
图1为原花青素结构通式。
图2为原花青素主要单体的结构；
图中，儿茶素(catechin,CT)，R1＝R2＝H，R3＝OH；表儿茶素(epicatechin,EC)，R1＝R3＝H，R2＝OH；棓儿茶素(gallocatechin,GC)，R2＝H，R1＝R3＝OH；表棓儿茶素(epigallocatechin,EGC)，R3＝H，R1＝R2＝OH；没食子酸表儿茶素酯(epicatechingallate,ECG)，R1＝R3＝H，R2＝G；没食子酸棓儿茶素酯(gallocatethingallate,GCG)，R2＝H，R1＝OH，R3＝G；没食子酸表棓儿茶素酯(epigallocatethingallate,EGCG)，R1＝R2＝OH，R2＝G。
图3为流动相的组成对原花青素各成分保留时间的影响。
图4为原花青素各成分HPLC色谱图；
图中，1.D6；2.C3；3.B2；4.EC；5.C1；6.D1；7.C2；8.D2；9.B5。
图5为酸梅汤未硫解前HPLC图。
图6为酸梅汤硫解HPLC的色谱图；
图中，1.表儿茶素；2.表儿茶素衍生物。
具体实施方式
为了便于理解本发明，下面将对本发明进行更全面的描述。但是，本发明可以以许多不同的形式来实现，并不限于本文所描述的实施例。相反地，提供这些实施例的目的是使对本发明的公开内容的理解更加透彻全面。
实施例1
一种酸梅汤，所述酸梅汤的制备原料包括如下重量份数的原料：山楂果120份、乌梅120份、甘草20份、陈皮60份、桂花10份。
所述酸梅汤的制备方法，按照如下步骤进行：
(1)按照重量份数，取山楂果120份、乌梅120份、甘草20份、陈皮60份，桂花10份，清洗干净；
(2)取洗净的山楂果和乌梅，加入8倍重量份数的水，熬煮锅中煮开后再熬煮30min；
(3)加入甘草和陈皮继续熬煮25min，再加入桂花继续熬煮5min；
(4)降温至室温捞渣，剩余液体过滤后加入占滤液质量3％的白砂糖，灌装杀菌制成；所述灌装杀菌为水浴杀菌，杀菌温度为95℃，杀菌时间30min。
实施例2
一种酸梅汤，所述酸梅汤的制备原料包括如下重量份数的原料：山楂果120份、乌梅120份、甘草20份、陈皮60份、桂花10份、越橘60份。
所述酸梅汤的制备方法，按照如下步骤进行：
(1)按照重量份数，取山楂果120份、乌梅120份、甘草20份、陈皮60份，桂花10份，清洗干净；
(2)取洗净的山楂果和乌梅，加入8倍重量份数的水，熬煮锅中煮开后再熬煮30min；
(3)加入甘草、陈皮和越橘继续熬煮25min，再加入桂花继续熬煮5min；
(4)降温至室温捞渣，剩余液体过滤后加入占滤液质量3％的白砂糖，灌装杀菌制成；所述灌装杀菌为水浴杀菌，杀菌温度为95℃，杀菌时间30min。
实验例：酸梅汤中原花青素类HPLC分析方法的建立及检测
原花青素类在280nm附近有最大吸收；试验以含23％(v/v)甲醇的水溶液为流动相A，含12％(v/v)乙腈的水溶液为流动相B，通过改变流动相配比，考察甲醇：乙腈的比例对各种多酚成分保留时间的影响，其变化规律如图3所示。由图3可见，当B％＝62％左右时(乙腈6.8％)，各原花青素类成分之间都实现了较好的分离，遂将流动相中甲醇和乙腈体积比确定为5:4(v/v)。
为了缩短洗脱时间，试验采用梯度洗脱的方式，即以水作A液，甲醇和乙腈体积比5:4(v/v)为B液，前期以15.4％的B液洗脱，以便使D6、C3、B2等得到较好的分离，随后提高流动相的洗脱强度，使后面的成分在保证分离效果的基础上缩短保留时间，最后用高洗脱强度的流动相将柱子中残留物洗出，平衡色谱柱。梯度洗脱程序为(min/B％)0/15.2，11/15.2，15/16.5，16/18，19/19.5，24/29，31/50，33/80，38/80，40/15.2，50/15.2。由于原花青素在含水的流动相中可部分电离，解离后极性增强，保留时间变短，峰形变宽，本试验采用甲酸500μL/L调节流动相的pH值。
采用以上的色谱条件对9种原花青素成分的标准品进行分析，图4为标准品的色谱图。如图4所示，原花青素各成分在该色谱条件下给出了单一的色谱峰，其纯度可以满足试验需要。
方法的回归方程、线性范围和最低检出限：分别取贮备液，用甲醇稀释，配制不同浓度的系列标准溶液，按所述色谱条件分析，以进样质量为自变量(X，μg)，峰面积为因变量(Y，mv·s)，分别求出各成分的线性回归方程、相关系数及线性范围。最低检出限以3倍信噪比(S/N)所对应的进样质量求得，结果列于表1。结果表明，响应值与进样质量之间线性关系良好，最低检出限在ng数量级，可以满足常规样品的定量分析。
表1 9种原花青素成分的回归方程、相关系数、线性范围及最低检出限
酸梅汤中的多酚类抗氧化活性成分主要是原花青素类成分，其组成的结构单元只有EC，在酸性条件下采用苄硫醚与之反应，最终可使聚合的原花青素彻底降解为表儿茶素苄硫醚(EC-S)以及末端单元的表儿茶素(EC)，这样便可以通过统计两者的含量来估计样品中原花青素的总含量及其平均聚合度。然而要实现以上分析目标，一个重要的前提就是要保证硫解反应必须彻底地定量完成，因此硫解反应条件的优化和控制就变得非常重要。本实施例以浓缩酸梅汤汁为试验材料，对硫解反应条件进行了优化试验，结果如下。
苄硫醇用量的优化按60μL浓缩10倍的酸梅汤、30μL酸(冰醋酸:1M盐酸＝50:1，v/v)与60μL苄硫醇溶液进行反应(保持总体积为150μL)，改变加入苄硫醇的浓度，使其在苄硫醇溶液中的浓度分别为1％、2％、3％、4％、5％、6％，反应温度为90℃，反应时间为60min，然后进样分析并统计EC和EC-S的峰面积。在150μL反应液中，随苄硫醇浓度的增加，原花青素单体EC及衍生物EC-S的峰面积总和逐渐增加，当苄硫醇的浓度达到5％时，EC与EC-S的面积总和达到最大，且继续增加苄硫醇浓度，硫解产物的峰面积基本保持不变，所以选择反应液中苄硫醇浓度为5％。
酸用量的优化：按照上述操作，保持加入酸的总量仍为30μL，改变其中醋酸与1M盐酸的配比，考察混酸的组成对PC降解和衍生效果的影响，当在冰醋酸中加入少量盐酸时，EC的峰面积变化并不明显，说明在冰醋酸条件下原花青素的降解反应已经能够完成，然而盐酸的添加对却使EC-S的峰面积明显增加，说明它有利于促进苄硫醚衍生物的生成。当混酸溶液中冰醋酸与盐酸的比例达到100:1-50:1时，EC-S的峰面积达到最高。然而当继续增加盐酸的含量时，发现EC-S和EC的峰面积均相应降低，这说明硫解反应产物在高酸性条件下并不稳定。为了确保所有样品中的聚合体都能较彻底反应，本试验选用混酸的比例为冰醋酸:1M盐酸＝50:1(v/v)。
硫解反应温度的影响温度会直接影响反应速率，当其他条件固定不变时，改变反应温度分别设80℃、85℃、90℃、95℃、100℃，观察其对衍生反应的影响，当水浴温度85℃和90℃时，反应进行得比较彻底，衍生产物含量达到最高，继续升高水浴温度，硫解产物的含量略有降低。为保证反应彻底，本实验采用了较温和的90℃的水浴温度。
硫解反应时间的优化：当确定了衍生剂浓度、酸液组成以及反应温度之后，PC的降解衍生反应的速率就已基本确定，所以通过延长反应时间就可以使衍生反应进行得足够彻底。按所述的条件操作，通过改变反应时间观察反应进行的程度，随反应时间的延长，EC的峰面积很快接近最高值且较稳定，而EC-S峰面积的增长表现得比较迟钝。经60min反应之后，硫解衍生物的总量达到最大值，继续延长反应时间其含量稍有下降。因此，本实验选用反应时间为60min。
综上所述，本实验确定的反应条件为：反应A液为5％(v/v)苄硫醇乙醇溶液，反应B液为冰醋酸:1M盐酸＝50:1(v/v)，于90℃下水浴反应时间60min。
采用上述优化的硫解-HPLC分析方法对实施例1和实施例2的酸梅汤(浓缩10倍)实际样品进行了原花青素总量的分析测定。首先采用所述的HPLC方法对实施例1的样品进样分析，结果见图5。从图中可以看到，未经过硫解反应的样品直接进样分析，其中的原花青素类成分主要以不同聚合度的聚合体的形式存在，由于成分太过复杂，彼此不能很好分离，尤其是图中15-19min的“馒头峰”，根本无法准确的统计峰面积。而同样的酸梅汤样品，经硫解衍生反应之后再进样分析，相同色谱条件下所得分析结果见图6，从中可以看到原来分布在15-19min之间的原花青素聚合物已经已经基本上被彻底降解，可以很方便的进行定量分析。
酸梅汤中9种多酚成分含量分析：
按上述分析方法对实施例1和实施例2的样品进行原花青素测定，测定结果见表2。由表2可以看出，实施例1中各原花青素含量差异较小，人体容易吸收利用的组分B2、EC和C1占比低于40％；而实施例2中容易吸收利用的组分B2、EC和C1占比较大，高于60％；实施例1与实施例2的差异在于实施例2的制备原料中多加入了越橘，证明越橘的加入，大幅提高了酸梅汤中容易被人体吸收利用的原花青素组分，对人体有益；发明人采用其他含有花青素的植物果实如桑葚、龙葵、葡萄、黑加仑、紫胡萝卜、红甘蓝替代越橘制备酸梅汤，B2、EC和C1组分在酸梅汤中均没有显著增加。
表2酸梅汤中原花青素组分含量(μg/g)
以上所述实施例仅表达了本发明的几种实施方式，其描述较为具体和详细，但并不能因此而理解为对发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。因此，本发明专利的保护范围应以所附权利要求为准。
Claims (7)
1.一种酸梅汤，其特征在于，所述酸梅汤的制备原料包括如下重量份数的原料：山楂果100-150份、乌梅100-150份、甘草10-30份、陈皮30-80份，桂花5-15份，越橘30-80份。
2.根据权利要求1所述酸梅汤，其特征在于，所述酸梅汤中的原花青素以EC、B2、C1为主，聚合程度低。
3.权利要求1所述酸梅汤的制备方法，其特征在于，按照如下步骤进行：
(1)按照重量份数，取山楂果100-150份、乌梅100-150份、甘草10-30份、陈皮30-80份，桂花5-15份，越橘30-80份，清洗干净；
(2)取洗净的山楂果和乌梅，加入3-15倍重量份数的水，熬煮锅中煮开后再熬煮20-35min；
(3)加入甘草、陈皮和越橘继续熬煮20-30min，再加入桂花继续熬煮3-6min；
(4)降温至室温捞渣，剩余液体过滤后加入占滤液质量1-6％的糖，灌装杀菌制成。
4.根据权利要求3所述酸梅汤的制备方法，其特征在于，所述糖为白砂糖、绵白糖或者红糖。
5.根据权利要求3所述酸梅汤的制备方法，其特征在于，所述灌装杀菌为水浴杀菌，杀菌温度为95℃，杀菌时间30min。
6.根据权利要求3所述酸梅汤的制备方法，其特征在于，所述酸梅汤的色泽为7580C-7600C。
7.根据权利要求3所述酸梅汤的制备方法，其特征在于，所述酸梅汤的PH为3.0-4.0；折光为12.0-14.0。
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6210681B1 (en) * | 1999-09-07 | 2001-04-03 | Jlb, Inc. | Plant proanthocyanidin extracts |
| CN101584488A (zh) * | 2009-06-22 | 2009-11-25 | 北京燕京饮料有限公司 | 纯天然酸梅汤及制造方法 |
| CN108991296A (zh) * | 2018-07-13 | 2018-12-14 | 宁夏金博乐食品科技有限公司 | 一种酸梅汤及其制备方法 |
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| US6210681B1 (en) * | 1999-09-07 | 2001-04-03 | Jlb, Inc. | Plant proanthocyanidin extracts |
| CN101584488A (zh) * | 2009-06-22 | 2009-11-25 | 北京燕京饮料有限公司 | 纯天然酸梅汤及制造方法 |
| CN108991296A (zh) * | 2018-07-13 | 2018-12-14 | 宁夏金博乐食品科技有限公司 | 一种酸梅汤及其制备方法 |
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