CN109602803A - 松葛降尿酸颗粒制备中柠檬苦素含量提高的方法 - Google Patents

松葛降尿酸颗粒制备中柠檬苦素含量提高的方法 Download PDF

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CN109602803A
CN109602803A CN201811561718.2A CN201811561718A CN109602803A CN 109602803 A CN109602803 A CN 109602803A CN 201811561718 A CN201811561718 A CN 201811561718A CN 109602803 A CN109602803 A CN 109602803A
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pueraria lobota
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loose
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阮晓
王强
杨丽
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Ningbo Institute of Technology of ZJU
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Abstract

本发明公开了松葛降尿酸颗粒制备中柠檬苦素含量提高的方法,用超临界萃取,其中夹带剂由乙醇、环己烷、水按照质量比范围7:1:2配制而成,该夹带剂可充分萃取柠檬苦素,甲醇吸收,吸收液用大孔树脂层析粗分离,得到淡黄色松葛降尿酸提取物135~145mg/100g,采用UPLC‑二极管阵列检测器标准物质外标法定量,提取物中柠檬苦素类的含量为35~40mg/g,本发明的提取方法简单,柠檬苦素提取充分,提取物也具有较强的降低尿酸水平的能力。

Description

松葛降尿酸颗粒制备中柠檬苦素含量提高的方法
技术领域
发明涉及中药颗粒剂制备中有效成分含量的提高方法,具体涉及松葛降尿酸颗粒制备中柠檬苦素含量提高的方法。
背景技术
高尿酸血症(Hyperuricemia,HUA)是一组以遗传性和(或)获得性体内嘌呤代谢紊乱和(或)尿酸(UA)排泄减少所导致的疾病。当富含嘌呤食物摄入过多、体内嘌呤生物合成障碍以及肾小管对尿酸盐的清除率降低时,均可出现循环血尿酸含量增高,导致高尿酸血症的发病。松葛降尿酸颗粒由松叶、葛根、陈皮三味中药组成,松叶为松科松属植物马尾松Pinus massoniana Lamb.的干燥叶,全年可采,除去杂质,晒干或低温干燥用,切成约4~10mm的段。葛根来源为:豆科植物野葛Pueraria lobata (Willd.)Ohwi的干燥根,习称野葛,秋、冬二季采挖,趁鲜切成边长约5~12mm的小块,干燥。陈皮来源为:芸香科植物橘Citrus reticulate Blanco及其栽培变种的干燥成熟果皮,药材分为“陈皮”和“广陈皮”,采摘成熟果实,剥取果皮,切丝,晒干或低温干燥。在浙江沿海地区尤其是宁波地区民间以袋泡茶形式服用,有祛风燥湿、清热解毒、健脾化痰之功效,主治痰湿阻滞(湿浊)、湿热内蕴型高尿酸血症。松葛降尿酸颗粒就是以松叶、葛根、陈皮经粉碎、提取有效成份,再加上药用辅料制备而成。
发明内容
本发明所要解决的技术问题是提供松葛降尿酸颗粒制备中柠檬苦素含量提高的方法,该方法提取简单,柠檬苦素提取充分,提取物中也具有较强的降低尿酸水平的能力。
本发明解决上述技术问题所采用的技术方案为:松葛降尿酸颗粒制备中柠檬苦素含量提高的方法,其步骤如下:
a、将松叶、葛根、陈皮按质量比4.5~4.75:4.5~4.75:0.5~1配制的松葛降尿酸颗粒粉碎后,过45~60目筛,得到松葛降尿酸粉末,装入超临界萃取釜中;
b、在超临界萃取釜中萃取,萃取温度为35~55℃,CO2流体压力为30~60MPa,夹带剂流速0.1~0.6ml/min,萃取时间2~4h,萃取物用甲醇吸收为吸收液,甲醇与原料松葛降尿酸粉末的体积质量比为1ml:2 g,所述夹带剂由乙醇、环己烷、水按照质量比范围7:1:2配制而成;该夹带剂可将药材中柠檬苦素类物质提取充分,其它物质提取相反有所降低;
c、吸收液用D101型大孔树脂层析,每小时两个柱床体积流速的蒸馏水洗脱至流出液无色,再用10个柱床体积的质量百分浓度60%乙醇洗柱子,乙醇洗脱液在450~500Pa条件下减压浓缩至近干,105℃干燥24h,得到淡黄色松葛降尿酸提取物。采用UPLC-二极管阵列检测器标准物质外标法定量,得到柠檬苦素含量较高的葛降尿酸提取物。柠檬苦素类含呋喃环三萜化合物成份主要为柠檬苦素、诺米林、脱乙酰诺米林、黄柏酮、米林酸,再与药用辅料配置成中药制剂松葛降尿酸颗粒。
与现有技术相比,本发明的优点在于松葛降尿酸颗粒制备中柠檬苦素含量提高的方法,用超临界萃取,其中夹带剂由乙醇、环己烷、水按照质量比范围7:1:2配制而成,该夹带剂可充分萃取柠檬苦素,甲醇吸收,吸收液用大孔树脂层析粗分离,得到淡黄色松葛降尿酸提取物135~145mg /100g,采用UPLC-二极管阵列检测器标准物质外标法定量,提取物中柠檬苦素类的含量为35~40mg/g,本发明的提取方法简单,柠檬苦素提取充分,提取物也具有较强的降低尿酸水平的能力。
具体实施方式
以下结合实施例对本发明作进一步详细描述。
实施例1
将松叶、葛根、陈皮按质量比4.5~4.75:4.5~4.75:0.5~1混合均匀100g,粉碎后,过45~60目筛,得到中药材粉末,装入超临界萃取釜中,在萃取温度为38℃,CO2流体压力为52MPa,夹带剂流速0.51ml/min,夹带剂由乙醇、环己烷、水按照质量比范围7:1:2配制而成;该夹带剂可将药材中柠檬苦素类物质提取充分,其它物质提取相反有所降低,萃取时间2.0h,萃取物用50ml甲醇吸收为吸收液,吸收液用D101型大孔树脂层析,每小时两个柱床体积流速的蒸馏水洗脱至流出液无色,再用10个柱床体积的质量百分浓度60%乙醇洗柱子,乙醇洗脱液在450~500Pa条件下减压浓缩至近干,105℃干燥24h,得到淡黄色松葛降尿酸提取物1.38g,采用UPLC-二极管阵列检测器标准物质外标法定量,提取物中柠檬苦素、诺米林、脱乙酰诺米林、黄柏酮、米林酸分别为12.4 mg/g、8.7 mg/g、9.2 mg/g、4.5 mg/g、4.2mg/g,提取物中柠檬苦素类含呋喃环三萜化合物的量共为39mg/g,因此柠檬苦素提取充分,再与药用辅料配置成中药制剂松葛降尿酸颗粒。
实施例2
与实施例1基本相同,所不同的只是萃取温度为35℃,CO2流体压力为30MPa,夹带剂流速0.1ml/min,萃取时间4h,得到淡黄色松葛降尿酸提取物1.35g,提取物中柠檬苦素类成分含量为36 mg/g。
实施例3
与实施例1基本相同,所不同的只是萃取温度为55℃,CO2流体压力为60MPa,夹带剂流速0.6ml/min,萃取时间2h,得到淡黄色松葛降尿酸提取物1.37g,提取物中柠檬苦素类成分含量为37 mg/g。
试验例1
对酵母膏+氧嗪酸钾致高尿酸血症模型小鼠的影响,采用连续灌胃给予酵母膏8天及末次腹腔注射氧嗪酸钾建立小鼠高尿酸血症模型,灌胃给予松葛降尿酸提取物(7.5 g提取物/kg、5.0 g提取物/kg、2.5 g提取物/kg),连续给药8天,松葛降尿酸提取物7.5g/kg能降低该高尿酸血症模型小鼠血清UA、Cr、BUN含量,降低血清及肝XOD、肝ADA活性,松葛降尿酸提取物5.0 g/kg能降低血清UA、Cr、BUN、TC、TG含量,降低血清XOD、血清及肝ADA活性,松葛降尿酸提取物2.5 g/kg能降低血清UA、BUN、TG含量,降低肝ADA活性。
试验例2
对黄嘌呤+乙胺丁醇致高尿酸血症小鼠模型的影响,采用连续灌胃给予黄嘌呤和乙胺丁醇16天建立小鼠高尿酸血症模型,灌胃给予松葛降尿酸提取物(7.5 g提取物/kg、5.0 g提取物/kg、2.5 g提取物/kg),连续给药16天,松葛降尿酸提取物三个剂量(7.5、5.0、2.5g/kg)能降低该模型小鼠血清UA、Cr、TG含量及AI,升高血清HDL-c含量。

Claims (2)

1.松葛降尿酸颗粒制备中柠檬苦素含量提高的方法,其特征在于步骤如下:
a、将松叶、葛根、陈皮按质量比4.5~4.75:4.5~4.75:0.5~1配制的松葛降尿酸颗粒粉碎后,过45~60目筛,得到松葛降尿酸粉末,装入超临界萃取釜中;
b、在超临界萃取釜中萃取,萃取温度为35~55℃,CO2流体压力为30~60MPa,夹带剂流速0.1~0.6ml/min,萃取时间2~4h,萃取物用甲醇吸收为吸收液,甲醇与原料松葛降尿酸粉末的体积质量比为1ml:2 g,所述夹带剂由乙醇、环己烷、水按照质量比范围7:1:2配制而成;
c、吸收液用D101型大孔树脂层析,每小时两个柱床体积流速的蒸馏水洗脱至流出液无色,再用10个柱床体积的质量百分浓度60%乙醇洗柱子,乙醇洗脱液在450~500Pa条件下减压浓缩至近干,105℃干燥24h,得到淡黄色松葛降尿酸提取物。
2.如权利要求1所述的松葛降尿酸颗粒制备中柠檬苦素含量提高的方法,其特征在于步骤b中,萃取温度为38℃,CO2流体压力为52MPa,夹带剂乙醇流速0.51ml/min,萃取时间2.0h。
CN201811561718.2A 2018-12-20 2018-12-20 松葛降尿酸颗粒制备中柠檬苦素含量提高的方法 Pending CN109602803A (zh)

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CN112755110A (zh) * 2020-11-25 2021-05-07 浙大宁波理工学院 芪珍胶囊中皂苷类物质含量提高的制备方法
CN114904364A (zh) * 2022-05-30 2022-08-16 万华化学集团股份有限公司 一种聚丙烯酸装置尾气处理方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112755110A (zh) * 2020-11-25 2021-05-07 浙大宁波理工学院 芪珍胶囊中皂苷类物质含量提高的制备方法
CN114904364A (zh) * 2022-05-30 2022-08-16 万华化学集团股份有限公司 一种聚丙烯酸装置尾气处理方法
CN114904364B (zh) * 2022-05-30 2024-04-09 万华化学集团股份有限公司 一种聚丙烯酸装置尾气处理方法

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