CN111298050B - 一种午时茶挥发油脂质体制备工艺、产品及其检测方法 - Google Patents
一种午时茶挥发油脂质体制备工艺、产品及其检测方法 Download PDFInfo
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Abstract
本发明公开了一种午时茶挥发油脂质体制备工艺,包括:以大豆磷脂为膜材,采用薄膜分散法对午时茶挥发油进行脂质体包裹,在成膜后利用去离子水进行水化,冻干得到所述午时茶挥发油脂质体。本发明还公开了一种午时茶挥发油脂质体产品,以及利用其制备午时茶颗粒的方法。本发明工艺简单易行,制备周期短,生产效率高,成本低,可用于大规模工业化生产。本发明方法与传统煎煮方法相适应,在提取过程中进行挥发油的收集,无需在提取前单独收集挥发油,能有效缩短提取时间、加快生产效率;同时应用挥发油脂质体包合技术,保证了午时茶颗粒在储存过程中挥发油的稳定性,提高了产品的质量和疗效。
Description
技术领域
本发明涉及中药制剂领域,具体涉及一种提高午时茶挥发油稳定性的制备工艺、产品及其成分检测方法。
背景技术
午时茶颗粒为《中国药典》收载品种,方剂源于清代《拔萃良方》中的天中茶,是由苍术、柴胡、羌活、防风、白芷、川芎、广藿香、前胡、连翘、陈皮、山楂、枳实、炒麦芽、甘草、桔梗、紫苏叶、厚朴、红茶、六神曲等19味中药组成的成方制剂,具有祛风解表,化湿中和的功效。组方中11味药可提取挥发油,成分十分复杂,具有发散解表、芳香开窍、祛风除湿、祛寒温里等功效。
现阶段生产企业针对午时茶颗粒制备工艺中挥发油的添加方式仍然以直接溶解喷洒加入法为主,该法虽简单易行,但由于挥发油是中药中的一类具有香气、挥发性、可随水蒸气蒸馏出来的重要的活性成分,在氧、光、热的作用下极易分解、变质而致稳定性较差,严重影响产品的质量及药效。
目前也有较多采用β-环糊精包裹挥发油的方式来解决上述存在的问题,但本发明的发明人研究发现β-环糊精包裹挥发油的午时茶产品在饮用时,当加入热水后会产生较大的挥发油刺鼻气味,原因是β原环糊精在热水中极易开环释放挥发油导致。刺鼻气味的产生,在一定程度上影响群众对该产品的接受度。
发明内容
综合以上存在的问题,本发明提供了一种采用包裹技术对午时茶挥发油进行包裹制备脂质体的方法。本发明同时再将午时茶挥发油脂质体加入到午时茶颗粒中,提供一种制备午时茶颗粒的方法。该方法一方面可防止午时茶挥发油挥发,提高挥发油的稳定性,保证产品的临床疗效;另一方面可掩盖挥发油的气味,弥补β-环糊精包裹挥发油的午时茶产品存在的缺点,将大大提高群众的接受度。
本发明对午时茶挥发油进行成分研究,发现其主要化学成分为α-蒎烯,β-蒎烯和d-柠檬烯。其中柠檬烯具有良好的镇咳、祛痰、平喘、抑菌、镇静中枢神经等作用,以d-柠檬烯为主要成分制成的复方柠檬烯胶囊,具有利胆溶石、理气开胃、消炎止痛的功效,可用于治疗胆结石、胆囊炎及胆道术后综合症等。蒎烯类物质具有良好的抗菌抗炎作用、抗痉挛活性和镇痛作用。但目前缺乏对午时茶挥发油的检测和质量控制研究。针对以上情况,本发明提供一种午时茶挥发油主要成分的检测方法。
本发明用于解决午时茶挥发油稳定性低、气味接受度差等问题。
为克服以上问题,本发明提供一种增加午时茶挥发油稳定性的制备工艺,包括:以大豆磷脂为膜材,采用薄膜分散法对午时茶挥发油进行脂质体包裹,在成膜后利用去离子水进行水化,冻干得到所述午时茶挥发油脂质体。
一种午时茶颗粒的制备方法,将上述方案或者下述任一方案得到的午时茶挥发油脂质体与午时茶初颗粒混匀,得到午时茶颗粒。
本发明的午时茶挥发油、午时茶初颗粒均可以按照药典记载的制备方法制备得到。比如所述午时茶挥发油可由如下方法制备得到:取苍术、柴胡、羌活、防风、白芷、川芎、广藿香、前胡、连翘、陈皮、枳实、紫苏叶、厚朴等13味中药(一个处方量700g,单个组份加入量按照药典加入)提取挥发油,蒸熘后的水溶液另器收集,备用;药渣与山楂、炒麦芽、甘草、桔梗、红茶、六神曲(炒)等6味中药加水煎煮二次,第一次2小时,第二次1小时,滤过,合并滤液,与上述水溶液合并,浓缩至相对密度为1.08~1.12(40~50℃)的清膏,加等量乙醇使沉淀,滤过,滤液回收乙醇并浓缩成稠膏,加蔗糖粉适量,制成颗粒,干燥,放冷,得到午时茶初颗粒。
作为优选的方案,一种午时茶挥发油脂质体制备工艺,包括如下步骤:
(1)将午时茶挥发油、大豆磷脂于乙醇中加热回流;
(2)将回流后的悬浮物在30~60℃下真空旋蒸,使均匀成膜;
(3)加入去离子水,25~60℃水化,成均匀乳状;
(4)冻干,得到午时茶挥发油脂质体。
作为优选,所述午时茶挥发油和大豆磷脂的重量比为1:3~1:8。进一步优选为1:4~1:6。大豆磷脂加入量,会明显影响午时茶挥发油的包裹率。步骤(1)中,可以首先按重量比混匀午时茶挥发油和磷脂,然后加入食用酒精,加入食用酒精的重量为午时茶挥发油、大豆磷脂总重量的4~10倍。作为进一步优选,食用酒精加入量为5~7倍量,可在较短时间内充分溶解大豆磷脂。
步骤(1)中,回流时间为2~6h。作为优选,加热回流最佳时间为4~5h,并进行搅拌。
步骤(2)中,作为优选,旋蒸的较佳温度为40~45℃,持续0.5~2h。挥发油损失量较低,成膜效果较好。转速为100~200r.min-1,进一步优选为100-150r.min-1。
步骤(2)中,通过时间和温度的控制,使得磷脂在旋蒸容器底部形成蜂窝状膜层结构,同时较低的温度同时降低了挥发油的挥发。步骤(3)中,利用水化过程,实现多层膜层的形成,进一步提高包裹率。
步骤(3)中,去离子水加入量为5~12倍,进一步优选为7~10倍,水化温度控制在35~45℃,水化时间为0.5~2h,进一步优选为,水化0.5~1h,得到的脂质体包封率较高。
步骤(4)中,冻干前,超声5~10min。
一种午时茶挥发油脂质体,由上述任一项技术方案所述的制备工艺制备得到。
作为优选,所述午时茶挥发油的主要化学成分包括α蒎烯、β蒎烯、柠檬烯、百秋李醇、紫苏醛等。
为保证产品质量与疗效,本发明提供了一种午时茶挥发油主要成分检测方法,具体方案为:一种午时茶挥发油成分的检测方法,所述方法包括气相色谱法。检测条件为:以(5%-苯基)-甲基聚硅氧烷(或极性相近)为固定液的毛细管柱为色谱柱,柱温:40℃保持7min,以3℃/min升温到85℃,以15℃/min升温到220℃并保持3min。进样口温度为250℃,检测器温度为260℃。
利用上述方法,可以直接实现对午时茶颗粒中挥发油主要成分检测,检测前可以利用现有方法首先实现对午时茶颗粒中挥发油的提取,然后对提取液利用上述方法进行检测。
本发明具有以下有益效果:
本发明工艺简单易行,制备周期短,生产效率高,成本低,可用于大规模工业化生产。
本发明方法与传统煎煮方法相适应,在提取过程中进行挥发油的收集,无需在提取前单独收集挥发油,能有效缩短提取时间、加快生产效率;同时应用挥发油脂质体包合技术,保证了午时茶颗粒在储存过程中挥发油的稳定性,提高了产品的质量和疗效。
另外通过该检测方法对比未包裹工艺生产的午时茶颗粒和包裹工艺生产的午时茶颗粒中挥发油的含量变化,发现脂质体包裹挥发油,不仅能提高午时茶颗粒中挥发油的稳定性,保证产品的质量和疗效,而且能改善产品的口感,提高群众对产品的接受度。
附图说明
图1为实施例中对午时茶颗粒中挥发油主要成分检测的气相色谱图;
图2为实施例中对照品的气相色谱图。
具体实施方式
为了使本发明的目的及优点更加清楚明确,以下结合实施例对本发明进行进一步阐述。应理解,此处所描述的具体实施例仅仅用以解释本发明,并不用于限制本发明的保护范围。
实施例1:午时茶颗粒制备
按照药典方法,取苍术、柴胡、羌活、防风、白芷、川芎、广藿香、前胡、连翘、陈皮、枳实、紫苏叶、厚朴等13味中药(一个处方量700g,物料量按照药典确定)提取挥发油,蒸熘后的水溶液另器收集,备用;药渣与山楂、炒麦芽、甘草、桔梗、红茶、六神曲(炒)等6味中药加水煎煮二次,第一次2小时,第二次1小时,滤过,合并滤液,与上述水溶液合并,浓缩至相对密度为1.08~1.12(40~50℃)的清膏,加等量乙醇使沉淀,滤过,滤液回收乙醇并浓缩成稠膏,加蔗糖粉适量,制成午时茶初颗粒,干燥,放冷,备用。
取大豆磷脂4.8g、挥发油1.2g于圆底烧瓶,按重量比加入6倍量的无水乙醇,于85℃加热回流1h,再置40℃真空120r.min-1旋蒸1h,均匀成膜。成膜后加48g去离子水,40℃水化1h,成稠乳状态,再置超声仪中超声8min,冻干,既得午时茶挥发油脂质体。将所制得的午时茶挥发油包合物均匀拌入上述干燥颗粒中,混匀即得午时茶颗粒。
经气相方法检测,午时茶挥发油提取率为0.17%,主要活性成分为α-蒎烯、β-蒎烯、柠檬烯、百秋李醇、紫苏醛等;采用紫外分光光度法检测(检测波长:334nm),午时茶挥发油脂质体包裹率为75%。
实施例2:
午时茶颗粒制粒方法与实施例1基本相同,所不同的在于挥发油包合工艺部分:取大豆磷脂7.2g、挥发油1.2g于圆底烧瓶,按重量比加入6倍量的无水乙醇,于85℃加热回流1h,再置40℃真空120r.min-1旋蒸1h,均匀成膜。成膜后加68g去离子水,40℃水化1h,成稠乳状态,再置超声仪中超声8min,冻干,既得午时茶挥发油脂质体。将所制得的午时茶挥发油包合物均匀拌入上述干燥颗粒中,混匀即得午时茶颗粒。
采用紫外分光光度法检测,午时茶挥发油脂质体包裹率为85%。
实施例3:午时茶挥发油成分检测
1、仪器与试剂:
Agilent 7890A
乙酸乙酯AR
2、色谱条件
色谱柱:(5%-苯基)-甲基聚硅氧烷(或极性相近)为固定液的毛细管柱
规格:30m*0.32mm*0.25μm
流量:1.5ml/min
分流比:10:1
温度:进样口温度为250℃;检测器温度为260℃
柱温:40℃(7min)-3℃/min-85℃-15℃/min-220℃(3min)
3、检测方法
对照品溶液制备:取α-蒎烯、β-蒎烯、柠檬烯对照品,加乙酸乙酯分别制成每1mL含α-蒎烯200μg、β-蒎烯400μg、柠檬烯400μg的溶液,作为对照品溶液。
供试品溶液制备:取(实施例1制备得到)午时茶颗粒18g,加240mL水,用挥发油提取法(甲法),提取2小时,收集油液至5mL量瓶中并用乙酸乙酯稀释至刻度,作为供试品溶液。
测定:取对照品溶液和供试品溶液分别直接进样1μL,记录色谱图谱。
供试品中应呈现3个特征峰,计算各特征峰与α-蒎烯、β-蒎烯、柠檬烯的保留时间,其保留时间应在各自规定值的±5%以内。对照品α-蒎烯、β-蒎烯、柠檬烯的保留时间的规定值分别为:14.14,16.48,19.41。
午时茶挥发油特征图谱见图1和图2:
对比例1
午时茶颗粒制粒方法与实施例1基本相同,所不同的在于挥发油包合工艺部分:取大豆磷脂1.2g、挥发油1.2g于圆底烧瓶,按重量比加入6倍量的无水乙醇,于85℃加热回流1h,再置40℃真空120r.min-1旋蒸1h,均匀成膜。成膜后加19.2g去离子水,40℃水化1h,成稠乳状态,再置超声仪中超声8min,冻干,既得午时茶挥发油脂质体。将所制得的午时茶挥发油包合物均匀拌入上述干燥颗粒中,混匀即得午时茶颗粒。
采用紫外分光光度法检测,午时茶挥发油脂质体包裹率为55%。
为验证脂质体包裹挥发油的稳定性,对样品中部分易挥发成分进行了稳定性试验,具体方案及结果如下:
(1)取供试品,批号为:20190117-1(直接喷入法:即采用现有方法将提取的挥发油直接喷洒到午时茶初颗粒上得到);20190117-2(实施例1制备得到)。
(2)供试品开口置蒸发皿中,摊开于60℃温度下放置10天,于第5天和第10天取样,按照上述检测方法,检测挥发油含量。(每个条件放置双份供试品)
(3)检测结果以0次的数值为100%,计算相对百分比含量,数据汇总见下表1。
表1
由表1可知,用传统喷洒工艺制备的得到的午时茶颗粒在60℃放置5天后,其中的α-蒎烯、α-蒎烯、柠檬烯显著降低,放置10天后,基本挥发完毕。而采用本发明的脂质体包裹方法处理挥发油,而后制备得到的午时茶颗粒,在60℃放置5天后其中的α-蒎烯、α-蒎烯、柠檬烯含量降低不明显,在在60℃放置10天后,含量依然保持在96%以上。
另外,采用申请号为2004100611707的专利文献(公开号为CN1650937A)的实施例7所述的方法,制备得到午时茶挥发油-β-环糊精包合物,并将午时茶挥发油-β-环糊精包合物与午时茶初颗粒混合均匀,得到β-环糊精包合物午时茶颗粒,作为与本发明实施例1制备得到的午时茶颗粒进行对比。将同样规格的上述两个样品加入到80~90℃的热水中,进行嗅觉检测,β-环糊精包合物午时茶颗粒加入热水后,会产生明显的挥发油刺鼻气味。而本发明制备的样品加入到80~90℃的热水中后,味道不明显,从嗅觉检测结果可知,本发明具有更好的接受度。
Claims (8)
1.一种午时茶挥发油脂质体制备工艺,其特征在于,以大豆磷脂为膜材,采用薄膜分散法对午时茶挥发油进行脂质体包裹,在成膜后利用去离子水进行水化,冻干得到所述午时茶挥发油脂质体,包括如下步骤:
(1)将午时茶挥发油、大豆磷脂于乙醇中加热回流;
(2)将回流后的悬浮物在40~45℃下真空旋蒸,使均匀成膜;
(3)加入去离子水,25~60℃水化,成均匀乳状;
(4)冻干,得到午时茶挥发油脂质体;
所述午时茶挥发油和大豆磷脂的重量比为1:3~1:8。
2.根据权利要求1所述的午时茶挥发油脂质体制备工艺,其特征在于,持续时间为0.5~2小时。
3.根据权利要求1所述的午时茶挥发油脂质体制备工艺,其特征在于,去离子水加入量为5~12倍,水化温度控制在35~45℃,水化时间为0.5~2h。
4.根据权利要求1所述的午时茶挥发油脂质体制备工艺,其特征在于,步骤(4)中,冻干前,超声5~10min。
5.一种午时茶挥发油脂质体,其特征在于,由权利要求1~4任一项所述的制备工艺制备得到。
6.根据权利要求5所述的午时茶挥发油脂质体,其特征在于,所述午时茶挥发油的主要化学成分包括α蒎烯、β蒎烯、柠檬烯、百秋李醇、紫苏醛中的一种或多种。
7.一种午时茶颗粒的制备方法,其特征在于,将权利要求1~4任一项所述的制备工艺制备得到午时茶挥发油脂质体与午时茶初颗粒混匀,得到午时茶颗粒;
所述午时茶初颗粒由下述方法制备得到:
取苍术、柴胡、羌活、防风、白芷、川芎、广藿香、前胡、连翘、陈皮、枳实、紫苏叶、厚朴13味中药提取挥发油,蒸熘后的水溶液另器收集,备用;药渣与山楂、炒麦芽、甘草、桔梗、红茶、六神曲6味中药加水煎煮二次,第一次2小时,第二次1小时,滤过,合并滤液,与上述水溶液合并,浓缩至相对密度为1.08~1.12的清膏,加等量乙醇使沉淀,滤过,滤液回收乙醇并浓缩成稠膏,加蔗糖粉适量,制成颗粒,干燥,放冷,得到午时茶初颗粒。
8.一种权利要求5或6所述的午时茶挥发油脂质体的检测方法,其特征在于,所述方法为气相色谱法,检测条件为:以(5%-苯基)-甲基聚硅氧烷为固定液的毛细管柱为色谱柱,柱温:40℃保持7min,以3℃/min升温到85℃,以15℃/min升温到220℃并保持3min,进样口温度为250℃,检测器温度为260℃。
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