CN105726574A - 玳瑁胶的制备及应用 - Google Patents
玳瑁胶的制备及应用 Download PDFInfo
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Abstract
本发明公开了一种玳瑁药材的炮制工艺，得到醋制玳瑁，能够明显提高玳瑁的有效成分提取率。本发明还公开了玳瑁胶的制备工艺，玳瑁胶具有和玳瑁相似的功效及应用范围，玳瑁胶便于携带便于服用。玳瑁经醋制及制成玳瑁胶后具有清热解毒、镇心安神的功效，可用于热病神昏、谵语惊狂、惊风抽搐、痈肿疮毒、斑疹症。玳瑁胶还可以制成保健品，用于改善或辅助改善心神不宁引起的失眠、多梦、不寐症状。本发明所用玳瑁为人工饲养品种。
Description
技术领域
本发明涉及玳瑁胶的制备及其应用，并公开玳瑁胶的制备方法，属于中药及中药制剂领域。
背景技术
玳瑁(EretmochelysimbricateLinnaeus)来源于龟鳖目Testudinata，潜颈龟亚目Cryptodira海龟科Cheloniidae玳瑁属Eretmochelys，背甲共有13块，作覆瓦状排列，所以又称十三鳞，古名瑇瑁，文甲等，中医药临床用其甲，具有清热解毒、镇心安神之功，可用于热病神昏、谵语惊狂、惊风抽搐、痈肿疮毒、斑疹等。早在唐代《本草拾遗》中就有记载，《本草纲目》谓：“玳瑁解毒清热之功同于犀角”，《圣惠方》载玳瑁丸，“治急风及中恶，不识人，面青，四肢逆冷”，《圣济总录》中玳瑁丸则“用于治疗中风不语，精神冒闷及中恶不语”。临床应用以生用为主，亦有炮制使用，炮制以蒸后镑极薄片及丝为主，《圣惠方》等文献中载有滑石粉制玳瑁的应用。临床研究发现玳瑁及其配方制剂能够改善癌症发热，还可用于免疫系统疾病、肺损伤等，临床应用多种药理活性。玳瑁甲片含有角蛋白、胶质、微量元素等，其体内所含的氨基酸种类和数量均较陆生龟鳖类高。
胶剂是指用动物皮、骨、甲、角等为原料，用水煎取胶质，浓缩成干胶状的内服制剂，其主要成分是动物水解蛋白类物质，并根据原料的特点加入一定量的冰糖、植物油、黄酒等辅料。目前，中医药临床使用的胶剂有阿胶、鹿角胶、龟甲胶、龟鹿二仙胶等。胶剂多以烊化内服为主，一般具有补益作用。中药玳瑁临床应用炮制品以净制、切制为主，偶有滑石粉制用。另外，玳瑁为国家二级保护动物，野生资源受国家保护，禁止捕捞使用。玳瑁分布范围较广，加勒比海地区、大洋洲海域、非洲海岸、印度洋海域等均有分布，中国从山东南部海域到南海诸岛海域均有分布，广东省及海南省部分地区有养殖，江苏、浙江、福建等沿海地区亦适合养殖，因此本发明所用玳瑁药材均来源于养殖品。
发明内容
本发明提供了一种新的玳瑁炮制工艺，得到醋制玳瑁，具体工艺如下。
本发明炮制工艺：取净河砂（过3号标准筛）120~180g，置炒药锅中翻炒至灵活状态、颜色加深，投入大小分档的玳瑁药材40~60g，翻炒至玳瑁甲片鼓起、有焦斑、酥脆、并有一定的甲焦臭味散出，起锅，筛去河砂，趁热投入米醋中，浸渍5~10分钟，捞出，控去醋液，30~70℃烘干。炒制过程中炉温控制在100~180℃，醋制时所用米醋量以能没过药材为度。
本发明提供了一种玳瑁胶剂的制备方法及工艺，制得玳瑁胶，其工艺如下。
本发明玳瑁胶的制备：玳瑁药材，打碎成大小均匀的块，洗净，取100g，加水2000~4000mL，常压，或加压1.2~1.6Mpa，温度100~110℃，煎煮5~24个小时，趁热过滤，滤渣如前述条件继续煎煮2~3次，合并滤液，加明矾0~0.1g，搅拌均匀，静置5~10个小时，滤取胶液。浓缩，待胶液浓缩去大部分水分后呈粘稠状态，加入豆油1~5ml，边加边搅拌至均匀无油泡。继续浓缩汁稠厚状态加入冰糖粉5~10g，黄酒5~10g，搅拌均匀，继续浓缩至胶液有气泡鼓起，挑起成片状或线状坠落，停止加热，趁热倒入事先涂抹植物油的瓷盘中，自然冷凝24~48个小时至成固体胶块，取出，切片，得玳瑁胶。玳瑁胶携带方便，服用方便，开水烊化服用即可。
本分明进一步提供玳瑁胶在中医药学上的应用，玳瑁胶在清热解毒、镇心安神功效上的应用，玳瑁胶可以用于高热神昏、谵语惊狂、惊风抽搐、痈肿疮毒、斑疹症。
本发明进一步提供玳瑁胶在保健品上的应用，玳瑁胶及含有玳瑁胶的糕点、糖果、饮品、保健品可以用于改善或辅助改善心神不宁等引起的失眠、不寐等症状。
具体实施方式
实施例1以70%的乙醇为溶剂按《中国药典》2015年版四部2201浸出物测定法项下热浸法测定不同炮制方法对玳瑁浸出物的影响，结果如下表所示。
| 玳瑁炮制品 | 生品 | 砂烫 | 蛤粉炒 | 滑石粉炒 | 砂烫醋淬 | 蛤粉炒醋淬 |
| 浸出物（%） | 7.34 | 10.16 | 10.36 | 8.62 | 18.89 | 12.16 |
炮制是根据中医药理论结合临床对中药进行的一系列加工处理，炮制可以使中药增效减毒、可以矫嗅矫味、利于有效成分的溶出。本实验通过对玳瑁浸出物的测定考察了炮制对玳瑁的影响，发现炮制后浸出物的量明显提高，加液体辅料米醋可以明显提高浸出物的量，其中砂烫醋淬后浸出物的量显著高于生品。对浸提方法的考察则发现热浸法较冷浸法可以得到更高的提取率。另外，炮制后玳瑁原有的腥臭味减失，更易于粉碎。
结论：通过浸出物的测定发现砂烫醋淬可以明显提高浸出物的量，以此为依据的话，砂烫醋淬为最佳提取工艺。
实施例2氨基酸的测定氨基酸测定色谱条件：洗脱泵流速0.45mL·min-1，衍生泵流速0.25mL·min-1，检测波长570nm、440nm，柱温58～74℃，反应器温度130℃，进样量50μl，流动相A为0.12N柠檬酸钠缓冲液（pH3.5）、流动相B为0.2N柠檬酸钠缓冲液（pH10.85）、流动相C为5%的甲醇水溶液用于检测后清洗色谱柱及仪器、流动相D为再生液、流动相配比如下表所示。
| 时间（min） | A% | B% | D% |
| 0.00～3.50 | 100 | 0 | 0 |
| 11.00 | 85 | 15 | 0 |
| 17.00 | 80 | 20 | 0 |
| 23.00 | 67 | 33 | 0 |
| 27.00～30.00 | 45 | 55 | 0 |
| 31.00～43.00 | 0 | 100 | 0 |
| 43.10～46.00 | 0 | 0 | 100 |
| 46.10～58.20 | 100 | 0 | 0 |
氨基酸对照品溶液的配制：天冬氨酸、苏氨酸、丝氨酸、谷氨酸、甘氨酸、丙氨酸、胱氨酸、缬氨酸、蛋氨酸、异亮氨酸、亮氨酸、酪氨酸、苯丙氨酸、组氨酸、赖氨酸、精氨酸、脯氨酸等17种氨基酸的混合对照品购至德国sykam公司，临用前稀释至0.2μmol·mL-1。
样品的处理-厌氧管充氮密封水解法：精密称取玳瑁（粉碎，过2号筛）约0.1g置厌氧水解管中，加入6mol·L-1的盐酸10mL，将样品全部浸没，冷冻10min，充高纯氮气2min，勿使液面溅起，移开氮气后立即密封，110±1℃水解22h。取出，放冷，精密量取0.3mL，60℃水浴氮气吹干，再精密加入样品稀释液2.00mL，滤过，取续滤液，即得。
样品含量测定：取3批玳瑁生品，按厌氧管充氮密封水解法制备样品溶液，分别进样，测定样品中17种氨基酸的含量，结果如下表所示。
| 氨基酸名称 | 含量% | RSD% |
| ASP天冬氨酸 | 2.27 | 0.8 |
| THR苏氨酸 | 1.27 | 0.8 |
| SER丝氨酸 | 4.17 | 0.0 |
| GLU谷氨酸 | 4.22 | 1.6 |
| PRO脯氨酸 | 8.27 | 0.5 |
| GLY甘氨酸 | 11.82 | 0.5 |
| ALA丙氨酸 | 1.78 | 0.6 |
| CYS胱氨酸 | 5.55 | 0.7 |
| VAL缬氨酸 | — | — |
| MET蛋氨酸 | 0.16 | 3.0 |
| ILE异亮氨酸 | 1.77 | 0.6 |
| LEU亮氨酸 | 6.80 | 0.3 |
| TYR酪氨酸 | 14.23 | 1.2 |
| PHE苯丙氨酸 | 2.71 | 2.1 |
| HIS组氨酸 | 3.39 | 2.1 |
| LYS赖氨酸 | 0.84 | 0.6 |
| ARG精氨酸 | 5.44 | 0.4 |
玳瑁经厌氧酸水解后测得氨基酸含量较高，总量不少于75%，其中酪氨酸、甘氨酸、脯氨酸、亮氨酸、胱氨酸、精氨酸等含量均大于5.00%，谷氨酸、丝氨酸、组氨酸、苯丙氨酸、天冬氨酸含量也大于2.00%，赖氨酸及蛋氨酸含量较少，缬氨酸未检出。
实施例3玳瑁糕的制备玳瑁胶100g，冰糖100g，核桃肉100g，桂圆肉30g，枸杞30g，黑芝麻100g，红枣100g,，熟莲子30g，黄酒200ml。冰糖置锅中加入黄酒煮至溶化，加入玳瑁胶烊化后，再依次加入核桃肉、桂圆肉、黑芝麻、红枣、莲子，文火熬制1~2小时，停止加热，倒入事先涂抹油脂的搪瓷盘中，放冷，切片。可用于改善失眠多梦不寐等症状。
以上实施例可以更详细说明本发明，但不以任何形式限制本发明。
Claims (5)
1.一种醋制玳瑁，其特征工艺如下：大小分档的玳瑁药材经砂烫后，河砂使用量是药材量的2至3倍，温度100～180℃；醋淬，醋的使用量浸没药材为度，醋浸时间5至10分钟，干燥制得。
2.根据权利要求1，醋制玳瑁在清热解毒、镇心安神功效上的应用，适用于热病神昏、谵语惊狂、惊风抽搐、痈肿疮毒、斑疹症。
3.一种玳瑁胶的制备，其工艺特征如下：玳瑁药材加水，温度100~110℃，煎煮5~24小时，过滤，滤液加明矾0%~0.1%，搅拌均匀，静置，滤取胶液，浓缩，再依次加入1%~5%的豆油，5%~10%的冰糖粉，5%~10%的黄酒，搅拌均匀，继续浓缩至胶液有气泡鼓起，挑起成片状或线状坠落，停止加热，趁热倒入事先涂抹植物油的瓷盘中，自然冷凝24~48个小时至成固体胶块，取出，切片，得玳瑁胶。
4.根据权利要求3，玳瑁胶在中医药学上的应用，具有清热解毒、镇心安神的功效，可用于高热神昏、谵语惊狂、惊风抽搐、痈肿疮毒、斑疹症。
5.根据权利要求3，玳瑁胶在保健品上的应用，玳瑁胶及含有玳瑁胶的糕点、糖果、饮品、保健品可以用于改善、辅助改善心神不宁引起的失眠、多梦、不寐症状。
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| CN109652565A (zh) * | 2019-02-13 | 2019-04-19 | 海南热带海洋学院 | 一种鉴别绿海龟和玳瑁制品的扩增引物及其应用和鉴别方法 |
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| CN106722258A (zh) * | 2016-11-18 | 2017-05-31 | 山东海葵生物科技有限公司 | 一种虾青素阿胶糕及其制备方法 |
| CN109652565A (zh) * | 2019-02-13 | 2019-04-19 | 海南热带海洋学院 | 一种鉴别绿海龟和玳瑁制品的扩增引物及其应用和鉴别方法 |
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