一种广藿香配方颗粒喷雾干燥方法Patchouli formula particle spray drying method
技术领域Technical field
本发明涉及中药配方颗粒生产技术领域,具体涉及一种改善的广藿香配方颗粒喷雾干燥方法,属于中药生产技术领域。The invention relates to the technical field of traditional Chinese medicine formula granule production, in particular to an improved spray-drying method of patchouli granules, belonging to the technical field of traditional Chinese medicine production.
背景技术Background technique
中药配方颗粒是由单味中药饮片经提取浓缩制成的、供中医临床配方用的颗粒。国内以前称单味中药浓缩颗粒剂,商品名及民间称呼还有免煎中药饮片、新饮片、精制饮片、饮料型饮片、科学中药等。The traditional Chinese medicine formula granules are prepared by extracting and concentrating the single-flavored traditional Chinese medicine decoction pieces for the clinical formula of Chinese medicine. Formerly known as single-flavor Chinese medicine concentrated granules, the name of the commodity and the folk name are also free of Chinese herbal medicine pieces, new pieces, refined pieces, beverage-type pieces, scientific Chinese medicine and so on.
干燥工艺是中药配方颗粒制备中的一个重要环节,中药浸膏干燥的方法有很多种,如真空干燥、冷冻干燥、流化床干燥、喷雾干燥等。其中,喷雾干燥具有干燥时间短、干燥面积大、有效成分破坏少等优点,是用于中药液态半液态物料干燥的一种较为理想的方法。The drying process is an important part in the preparation of Chinese medicine formula granules. There are many methods for drying traditional Chinese medicine extracts, such as vacuum drying, freeze drying, fluidized bed drying, spray drying and the like. Among them, spray drying has the advantages of short drying time, large drying area and less damage of active ingredients, and is an ideal method for drying liquid semi-liquid materials of traditional Chinese medicine.
中药广藿香为唇形科植物广藿香Pogostemon cablin(Blanco)Benth.的干燥地上部分。具有芳香化浊,和中止呕,发表解暑的功效,主要用于治疗湿浊中阻,脘痞呕吐,暑湿表证,湿温初起,发热倦怠,胸闷不舒,寒湿闭暑,腹痛吐泻,鼻渊头痛。The Chinese herb patchouli is the dry aerial part of the Pogostemon cablin (Blanco) Benth. It has the effect of aromatizing turbidity, and stopping vomiting, and releasing the effect of relieving heat. It is mainly used for the treatment of wet turbidity, vomiting, phlegm, phlegm, dampness, fever, burnout, chest tightness, cold and dampness. Abdominal pain, vomiting and diarrhea, nasal headache.
广藿香作为中药配方颗粒使用已经是现有技术,但关于广藿香配方颗粒干燥技术的公开的内容较少。中国发明专利申请(CN107397787A)公开了一种广藿香鲜榨喷雾干燥颗粒饮片的制备工艺,其将压榨得到的广藿香药汁于40~80℃减压浓缩,得到相对密度为1.02~1.10的浓缩液,然后进行喷雾干燥,进风口温度设定为100~140℃,出风口温度设定为90~120℃条件下直接进行喷雾干燥。CN107397787A中公开的方法尽管简单易操作,但由于广藿香中含有各种醇、酮、糖苷等成分,会因为料液粘度较大,造成药液在在喷雾干燥过程中粘塔现象,不仅严重影响喷雾干燥效率,还会损失部分物料、降低干膏粉的收率。It has been a prior art to use patchouli as a Chinese medicine formula granule, but there is less disclosure about the patchouli granule drying technique. The Chinese invention patent application (CN107397787A) discloses a preparation process of a patchouli fresh-squeezed spray-dried granules, which concentrates the pressed patchouli medicinal juice under reduced pressure at 40-80 ° C to obtain a relative density of 1.02 to 1.10. The concentrated liquid is then spray dried, and the air inlet temperature is set to 100 to 140 ° C, and the outlet temperature is set to 90 to 120 ° C, and spray drying is directly performed. Although the method disclosed in CN107397787A is simple and easy to operate, since the patchouli contains various alcohols, ketones, glycosides and the like, the viscosity of the liquid is large, which causes the liquid to stick to the tower during the spray drying process, which is not only serious. Affecting spray drying efficiency, it will also lose some materials and reduce the yield of dry paste powder.
发明内容Summary of the invention
技术问题technical problem
本发明的目的在于克服现有技术的不足,提供一种工艺简单利于工业化生产、能够有效防止喷雾干燥过程中的粘壁现象、且有效提高中药浸膏在喷雾干燥过程中干膏粉收率的广藿香中药配方颗粒喷雾干燥工艺。The object of the present invention is to overcome the deficiencies of the prior art, to provide a process which is simple for industrial production, can effectively prevent the sticking phenomenon in the spray drying process, and effectively improve the yield of the dry paste powder in the spray drying process of the traditional Chinese medicine extract. Patchouli Chinese Herbal Formula Granule Spray Drying Process.
解决方案solution
为了解决上述技术问题,本发明所采用的技术方案是:In order to solve the above technical problems, the technical solution adopted by the present invention is:
一种广藿香中药配方颗粒喷雾干燥方法,所述方法包含如下步骤:取浓缩后的广藿香浸膏,然后加入2%~5%倍他环糊精,混匀,滤过,在进风温度175℃~180℃,出风温度90℃~95℃条件下进行喷雾干燥,收集干膏粉。A method for spray drying a patchouli Chinese medicine formula, the method comprising the steps of: taking a concentrated patchouli extract, then adding 2% to 5% beta cyclodextrin, mixing, filtering, and advancing The air temperature was 175 ° C to 180 ° C, and the air temperature was 90 ° C to 95 ° C under spray drying to collect the dry paste powder.
如上所述的喷雾干燥方法,作为一种优选方式,其中所述浓缩后的浸膏在60℃相对密度为1.02至1.10,优选为1.03至1.10。The spray drying method as described above, as a preferred mode, wherein the concentrated extract has a relative density of from 1.02 to 1.10, preferably from 1.03 to 1.10 at 60 °C.
如上所述的喷雾干燥方法,作为一种优选方式,其中所述浓缩后的浸膏在60℃相对密度为1.05至1.08。As the spray drying method as described above, as a preferred mode, the concentrated extract has a relative density of 1.05 to 1.08 at 60 °C.
如上所述的喷雾干燥方法,作为一种优选方式,其中浸膏加入3%~4%的倍他环糊精。优选加入3%的倍他环糊精。As the spray drying method as described above, as a preferred embodiment, the extract is added with 3% to 4% of betacyclodextrin. Preferably, 3% beta-cyclodextrin is added.
如上所述的喷雾干燥方法,作为一种优选方式,喷雾干燥中的进风温度为175℃,出风温度为95℃。As the spray drying method as described above, as a preferred mode, the inlet air temperature during spray drying is 175 ° C, and the outlet air temperature is 95 ° C.
如上所述的喷雾干燥方法,作为一种优选方式,其中所述干膏收率为78.02%~96.56%,优选为78.02%、81.09%、81.15%、84.57%、95.44%或96.56%。As a preferred embodiment, the spray drying method has a dry paste yield of 78.02% to 96.56%, preferably 78.02%, 81.09%, 81.15%, 84.57%, 95.44% or 96.56%.
作为常用的计量方式,本申请中倍他环糊精的加入量是以浓缩后的广藿香浸膏的重量为基准来计算的。As a commonly used metering method, the amount of beta-cyclodextrin added in the present application is calculated based on the weight of the concentrated patchouli extract.
发明人通过多年对中药配方颗粒喷雾干燥的研究,惊奇的发现,在制备广藿香配方颗粒时,只需加入少量倍它环糊精作为广藿香配方颗粒喷雾干燥的辅料,即可极大改善喷雾干燥过程中的粘塔现象,极大地提高广藿香配方颗粒喷雾干燥过程中的干膏收率。现有技术一般认为倍他环糊精作为常用的药用辅料,主要用于挥发油的包合,而较少作为喷雾干燥的辅料,少量文献报道其使用的用量也在5%以上,而辅料用量过多,不仅影响配方颗粒中主药的含量,增加病人服用量,还会造成工业化生产中的成本增大等不利效果。同时申请人还发现,广藿香浸膏的相对密度同样是影响喷雾干燥工艺及干膏收率的一大因素,相对密度过大或过小均会影响喷雾干燥情况及干膏收率,相对密度处于合适范围利于喷雾干燥过程中的工艺控制及干膏粉收率。After many years of research on the spray drying of traditional Chinese medicine formula particles, the inventors have surprisingly found that in the preparation of patchouli granules, it is only necessary to add a small amount of cyclodextrin as a spray-dried excipient for patchouli granules. Improve the sticking tower phenomenon during spray drying, and greatly improve the dry paste yield during the spray drying process of patchouli formula particles. The prior art generally considers beta-cyclodextrin as a commonly used pharmaceutical excipient, mainly used for the inclusion of volatile oils, and less as an auxiliary material for spray drying, and a small amount of literature reports that the amount used is also more than 5%, and the amount of auxiliary materials. Excessive, not only affects the content of the main drug in the formula granules, increases the dosage of the patient, but also causes an unfavorable effect such as an increase in cost in industrial production. At the same time, the applicant also found that the relative density of patchouli extract is also a major factor affecting the spray drying process and dry paste yield. If the relative density is too large or too small, it will affect the spray drying condition and dry cream yield. The density is in the proper range to facilitate process control and dry paste powder yield during spray drying.
具体实施方式detailed description
下面通过实施例对本发明做进一步详细说明,这些实施例仅用来说明本发明,并不限制本发明的范围。The invention is further illustrated by the following examples, which are intended to illustrate the invention and not to limit the scope of the invention.
实施例1Example 1
取浓缩后的广藿香浸膏,相对密度为1.05(60℃),在进风温度175℃,出风温度95℃条件下进行喷雾干燥,收集干膏粉。The concentrated patchouli extract was taken to have a relative density of 1.05 (60 ° C), spray-dried at an inlet air temperature of 175 ° C, and an outlet air temperature of 95 ° C to collect dry paste powder.
实施例2Example 2
取浓缩后的广藿香浸膏,相对密度为1.05(60℃),然后加入2%倍他环糊精,混匀,滤过,在进风温度175℃,出风温度95℃条件下进行喷雾干燥,收集干膏粉。Take the concentrated patchouli extract, the relative density is 1.05 (60 ° C), then add 2% beta cyclodextrin, mix, filter, at the inlet air temperature of 175 ° C, the outlet temperature of 95 ° C Spray dry and collect dry paste powder.
实施例3Example 3
取浓缩后的广藿香浸膏,相对密度为1.05(60℃),然后加入3%倍他环糊精,混匀,滤过,在进风温度175℃,出风温度95℃条件下进行喷雾干燥,收集干膏粉。The concentrated patchouli extract was obtained at a relative density of 1.05 (60 ° C), then added with 3% cyclodextrin, mixed, filtered, and subjected to an inlet air temperature of 175 ° C and an outlet temperature of 95 ° C. Spray dry and collect dry paste powder.
实施例4Example 4
取浓缩后的广藿香浸膏,相对密度为1.05(60℃),然后加入4%倍他环糊精,混匀,滤过,在进风温度175℃,出风温度95℃条件下进行喷雾干燥,收集干膏粉。The concentrated patchouli extract was taken at a relative density of 1.05 (60 ° C), then 4% beta-cyclodextrin was added, mixed, filtered, and subjected to an inlet air temperature of 175 ° C and an outlet air temperature of 95 ° C. Spray dry and collect dry paste powder.
实施例5Example 5
取浓缩后的广藿香浸膏,相对密度为1.03(60℃),然后加入3%倍他环糊精,混匀,滤过,在进风温度175℃,出风温度95℃条件下进行喷雾干燥,收集干膏粉。The concentrated patchouli extract was taken at a relative density of 1.03 (60 ° C), then 3% times cyclodextrin was added, mixed, filtered, and subjected to an inlet air temperature of 175 ° C and an outlet temperature of 95 ° C. Spray dry and collect dry paste powder.
实施例6Example 6
取浓缩后的广藿香浸膏,相对密度为1.08(60℃),然后加入3%倍他环 糊精,混匀,滤过,在进风温度175℃,出风温度95℃条件下进行喷雾干燥,收集干膏粉。Take the concentrated patchouli extract, the relative density is 1.08 (60 ° C), then add 3% times cyclodextrin, mix, filter, at the inlet air temperature of 175 ° C, the outlet temperature of 95 ° C Spray dry and collect dry paste powder.
实施例7Example 7
取浓缩后的广藿香浸膏,相对密度为1.10(60℃),然后加入3%倍他环糊精,混匀,滤过,在进风温度175℃,出风温度95℃条件下进行喷雾干燥,收集干膏粉。Take the concentrated patchouli extract, the relative density is 1.10 (60 ° C), then add 3% times cyclodextrin, mix, filter, at the inlet air temperature of 175 ° C, the outlet temperature of 95 ° C Spray dry and collect dry paste powder.
实施例8Example 8
取浓缩后的广藿香浸膏,相对密度为1.01(60℃),然后加入3%倍他环糊精,混匀,滤过,在进风温度175℃,出风温度95℃条件下进行喷雾干燥,收集干膏粉。The concentrated patchouli extract was taken at a relative density of 1.01 (60 ° C), then 3% times cyclodextrin was added, mixed, filtered, and subjected to an inlet air temperature of 175 ° C and an outlet air temperature of 95 ° C. Spray dry and collect dry paste powder.
实施例9Example 9
取浓缩后的广藿香浸膏,相对密度为1.11(60℃),然后加入3%倍他环糊精,混匀,滤过,在进风温度175℃,出风温度95℃条件下进行喷雾干燥,收集干膏粉。The concentrated patchouli extract was taken at a relative density of 1.11 (60 ° C), then 3% times cyclodextrin was added, mixed, filtered, and subjected to an inlet air temperature of 175 ° C and an outlet temperature of 95 ° C. Spray dry and collect dry paste powder.
实施例10Example 10
取浓缩后的广藿香浸膏,相对密度为1.05(60℃),然后加入1.5%倍他环糊精,混匀,滤过,在进风温度175℃,出风温度95℃条件下进行喷雾干燥,收集干膏粉。The concentrated patchouli extract was taken at a relative density of 1.05 (60 ° C), then 1.5% beta-cyclodextrin was added, mixed, filtered, and subjected to an inlet air temperature of 175 ° C and an outlet temperature of 95 ° C. Spray dry and collect dry paste powder.
实施例11Example 11
取浓缩后的广藿香浸膏,相对密度为1.05(60℃),然后加入6%倍他环糊精,混匀,滤过,在进风温度175℃,出风温度95℃条件下进行喷雾干燥,收集干膏粉。Take the concentrated patchouli extract, the relative density is 1.05 (60 ° C), then add 6% times cyclodextrin, mix, filter, at the inlet air temperature of 175 ° C, the outlet temperature of 95 ° C Spray dry and collect dry paste powder.
喷雾干燥情况及干膏收率考察结果Spray drying condition and dry cream yield inspection results
表1Table 1
实施例Example
|
喷雾干燥情况Spray drying
|
干膏收率(%)Dry paste yield (%)
|
11
|
粘塔,干膏粉流动性差Sticky tower, dry paste powder has poor fluidity
|
65.4065.40
|
22
|
略粘塔,干膏粉流动性一般Slightly sticky tower, dry paste powder is generally fluid
|
81.1581.15
|
33
|
不粘塔,干膏粉流动性好Non-stick tower, dry paste powder has good fluidity
|
95.4495.44
|
44
|
不粘塔,干膏粉流动性好Non-stick tower, dry paste powder has good fluidity
|
84.5784.57
|
55
|
略粘塔,干膏粉流动性一般Slightly sticky tower, dry paste powder is generally fluid
|
81.0981.09
|
66
|
不粘塔,干膏粉流动性好Non-stick tower, dry paste powder has good fluidity
|
96.5696.56
|
77
|
略粘塔,干膏粉流动性一般Slightly sticky tower, dry paste powder is generally fluid
|
78.0278.02
|
88
|
粘塔,干膏粉流动性差Sticky tower, dry paste powder has poor fluidity
|
70.6570.65
|
99
|
粘塔,干膏粉流动性差Sticky tower, dry paste powder has poor fluidity
|
71.1171.11
|
1010
|
粘塔,干膏粉流动性差Sticky tower, dry paste powder has poor fluidity
|
72.9772.97
|
1111
|
粘塔,干膏粉流动性差Sticky tower, dry paste powder has poor fluidity
|
71.4571.45
|
从考察结果可以看出,干膏粉浓缩后的相对密度与是否使用辅料倍他环糊精及使用倍他环糊精的量对喷雾干燥过程及干膏收率有很大影响,相对密度为1.05-1.08,倍他环糊精的用量在3%左右,喷雾干燥情况最好,干膏收率最高。It can be seen from the results of the investigation that the relative density of the dry paste powder after concentration and the use of the excipient beta-cyclodextrin and the amount of beta-cyclodextrin have a great influence on the spray drying process and the dry paste yield, and the relative density is 1.05-1.08, the dosage of beta-cyclodextrin is about 3%, the best spray drying, the highest dry cream yield.