A low-toxic and high-efficiency processing technology for Heishun tablets

Abstract

The present invention relates to a low-toxic and high-efficiency Heishun tablet preparation process, which includes the following main steps: (i) washing and pickling; (ii) steaming and slicing; (iii) soaking and bleaching; (iv) reducing toxicity and increasing efficacy: adding wine yeast and jujube juice to the soaked and bleached aconite tablets, and keeping the temperature at 25-40°C for 48-72 hours; (v) drying. Compared with the prior art, (1) the salt pickling method used in the present invention not only plays a role in the preservation of aconite but is also safe and reliable; (2) the nutrients in the jujube juice can allow the Aspergillus in the wine yeast to grow well. The wine yeast and its products can convert diester alkaloids in the aconite tablets into monoester alkaloids in an ethanol aqueous solution environment and avoid excessive hydrolysis of diester alkaloids to greatly weaken the efficacy; (3) jujube is a sweet, slow, nourishing and soft product that can alleviate the medicinal properties of aconite, reduce the toxicity of aconite and improve the efficacy; (4) the jujube juice can make the surface color of the product Heishun tablets yellow-brown and transparent, and can achieve the color enhancement effect of Heishun tablets while reducing toxicity and increasing efficacy.

Description

Technical Field

[0001] The invention relates to the technical field of processing of traditional Chinese medicine Heishunpian, in particular to a low-toxic and high-efficiency processing technology of Heishunpian. Background Art

[0002] Heishunpian, also known as processed aconite, is the rhizome of Aconitum, which mainly contains aconite alkaloids and some polysaccharides and lipids. Heishunpian has the effects of dispelling wind and dampness, tonifying the kidney and strengthening yang, dispelling cold and relieving pain. It can treat wind-cold dampness, impotence due to kidney deficiency, abdominal pain due to cold hernia, cold pain in the heart and abdomen, dysmenorrhea, palpitations, abdominal distension and pain, cold and cold, etc. It is called "the first product for restoring yang and rescuing adverse conditions". However, aconite is poisonous. Unprocessed aconite is more toxic and needs to be used with caution. Although the aconite processed by traditional technology (Heishunpian) has reduced its toxicity to a certain extent, it is still more toxic and the effective ingredients are easily lost. According to research, the main pharmacologically active ingredients of Heishun Tablets are monoester and diester alkaloids (aconitine), which are the most active. The diester alkaloids are highly toxic and can easily lead to moderate or even death. The traditional processing method hydrolyzes the diester alkaloids into monoester alkaloids by steaming to reduce toxicity, but the traditional processing method cannot control the degree of hydrolysis well, and it is easy to have a low degree of hydrolysis and high drug toxicity or an excessive degree of hydrolysis. Most of the monoester alkaloids and diester alkaloids are hydrolyzed into alcoholamine alkaloids and lose most of their medicinal properties. At present, there are also different technologies that control the degree of hydrolysis as much as possible by controlling the steaming time and temperature, such as a processing method of Heishun Tablets in a Chinese patent document with publication number CN 114917276 A. This method can achieve quantitative and standardized operation to a certain extent, but it still fails to solve the problem of how to effectively reduce the hydrolysis of diester alkaloids into monoester alkaloids while preventing excessive hydrolysis.

[0003] A Chinese document with publication number CN 101434577 B discloses a method for converting diester-type and lipid-type alkaloids in a Chinese herbal medicine of the genus Aconitum into monoester-type alkaloids, wherein Chinese herbal medicine powder is put into 1,4-dioxane and refluxed in a water bath at 95-100° C. for 6-24 hours to convert diester-type alkaloids into monoester-type alkaloids. Although this method reduces the original toxicity of the Chinese herbal medicine, it introduces a new harmful substance, 1,4-dioxane, which is also known as 1,4-dioxane and is a Class 2B carcinogen.

[0004] Therefore, in view of the problems existing in the prior art, there is an urgent need to provide a processing technology that effectively reduces the toxicity of aconite, prevents the effective ingredients from being lost, and is safe and reliable. Summary of the invention

[0005] The purpose of the present invention is to avoid the shortcomings of the prior art and provide a low-toxic, high-efficiency, safe and reliable method for preparing Heishun tablets.

[0006] The purpose of the present invention is achieved through the following technical solutions:

[0007] Provided is a low-toxic and high-efficiency Heishun tablets preparation process, comprising the following main steps:

[0008] 1. Wash and marinate

[0009] Clean the aconite root, drain the water and marinate it with sodium chloride until it becomes hard and has salt crystals on the surface;

[0010] 2. Steaming and slicing

[0011] Put the aconite root into water and cook it at a constant temperature for 8-12 hours, and control the temperature at 50-80℃;

[0012] Slice the steamed aconite for later use;

[0013] (III) Soaking and bleaching

[0014] Put the aconite slices processed in step (ii) into water for soaking;

[0015] (IV) Reducing toxicity and increasing efficacy

[0016] Add wine yeast and jujube juice to the soaked and bleached aconite tablets, and treat at a constant temperature of 25-40°C for 48-72 hours;

[0017] (V) Drying

[0018] The aconite slices processed in step (iv) are placed in an oven for drying.

[0019] Preferably, in step (iv), 8-20 g of wine yeast and 250-400 g of jujube juice are added per kilogram of aconite tablets; the preparation method of jujube juice is as follows:

[0020] After removing the core of the jujube, add water to pulp and filter to obtain the filtrate, wherein 2-3 kg of water is added for every kilogram of jujube.

[0021] Preferably, in step (i), the aconite root is cleaned and drained for later use, a layer of coarse salt is spread on the bottom of the pickling container, followed by a layer of aconite root, and then a layer of coarse salt, and the like is arranged at intervals; after pickling, the undissolved coarse salt is recovered and reused.

[0022] Preferably, in step (ii), the aconite root is directly sliced ​​or peeled and then sliced.

[0023] Preferably, in step (iii), the aconite tablets are soaked in water for 2 to 3 hours each time, and the water is changed; the soaking is performed 2 to 3 times in total.

[0024] Preferably, in step (v), the drying time is 2 to 5 hours.

[0025] Preferably, in step (v), the drying method is staged heating drying: placing the aconite slices in an oven, maintaining the temperature at 50-80°C for drying for 30-90 minutes, heating to 80-110°C for drying for 60-120 minutes, and heating to 110-140°C for drying for 30-90 minutes.

[0026] Preferably, in step (v), the pressure in the oven is 1.2×10 5 ~1.5×10 5 pa.

[0027] Preferably, in step (i), the aconite is cleaned and drained and then pickled with sodium chloride for 12 to 48 hours.

[0028] Compared with the prior art, the present invention has the following major outstanding improvements:

[0029] The method of pickling with salt is adopted instead of soaking in bile water solution for preservation. Bile water is commonly known as brine, which mainly consists of magnesium chloride, magnesium sulfate and sodium chloride. Brine is toxic. After magnesium ions are absorbed, they can inhibit the cardiovascular and nervous systems. The method of pickling with salt used in the present invention not only has the effect of preserving aconite but is also safe and reliable.

[0030] After slicing, add koji and jujube juice. The koji can convert starch, sugar and other substances in the jujube juice into a mixture containing ethanol. The nutrients in the jujube juice can allow the Aspergillus in the koji to grow well. The koji and its products can convert the diester alkaloids in the aconite tablets into monoester alkaloids in an ethanol-water solution environment. The process of converting diester alkaloids into monoester alkaloids mainly includes hydrolysis and alcoholysis of diester alkaloids. The degree of hydrolysis in this process is inhibited to a certain extent. The diester alkaloids will not be over-hydrolyzed to generate aconitine and the like, which greatly weakens the efficacy, thereby increasing the conversion rate of diester alkaloids into monoester alkaloids, effectively reducing toxicity and improving efficacy.

[0031] Jujube is a sweet, slow and nourishing food. It can not only nourish the spleen and stomach, nourish the blood and calm the mind, but also moderate the medicinal properties. It can well moderate the active and urgent medicinal properties of aconite, reduce its toxicity, coordinate yin and yang, and improve the efficacy.

[0032] Jujube juice is rich in sugar, which seeps into the aconite tablets and adheres to the outside. When dried, the final product, Heishun tablets, can have a translucent yellow-brown appearance, which can achieve the color enhancement effect of Heishun tablets while reducing toxicity and increasing efficacy. Implementation

[0033] The present invention will be further described with reference to the following examples. Example 1

[0034] The low-toxic and efficient Heishun tablets processing technology of the present embodiment mainly comprises the following steps:

[0035] 1. Wash and marinate

[0036] Clean the aconite root, drain the water, and then marinate it with sodium chloride until it becomes hard and salt crystals appear on the surface; in this embodiment, marinate for 25 hours.

[0037] 2. Steaming and slicing

[0038] Put the aconite root into water and cook it at a constant temperature of 65℃ for 10h;

[0039] Slice the steamed aconite for later use;

[0040] (III) Soaking and bleaching

[0041] Put the aconite slices processed in step (ii) into water for soaking;

[0042] (IV) Reducing toxicity and increasing efficacy

[0043] Adding wine yeast and jujube juice to the soaked and bleached aconite slices, and treating at a constant temperature of 30°C for 50 hours;

[0044] Among them, 15g of wine yeast and 300g of jujube juice are prepared for each kilogram of aconite tablets; the preparation method of jujube juice is as follows:

[0045] After removing the core of the jujube, add water to pulp and filter to obtain the filtrate, wherein 2.5 kg of water is added for every kilogram of jujube.

[0046] (V) Drying

[0047] The aconite tablets treated in step (iv) are placed in an oven for drying at a temperature of 100 degrees Celsius for 2 hours. The drying time in step (v) of the present invention may also be 4 hours or 5 hours, as long as the drying effect is achieved so that the Heishun tablets can be dried and stored for a long time. Example 2

[0048] The main technical scheme of this embodiment is basically the same as that of Embodiment 1. For features not explained in this embodiment, the explanation in Embodiment 1 is adopted and will not be repeated here. The difference between this embodiment and Embodiment 1 is that:

[0049] Step (V) Drying method is segmented heating drying: Place the aconite slices in an oven, maintain the temperature at 65°C for drying for 60 minutes, increase the temperature to 90°C for 90 minutes, and increase the temperature to 125°C for drying for 60 minutes. Example 3

[0050] The main technical scheme of this embodiment is basically the same as that of Embodiment 1. For features not explained in this embodiment, the explanation in Embodiment 1 is adopted and will not be repeated here. The difference between this embodiment and Embodiment 1 is that:

[0051] Step (V) Pressurized drying, the pressure in the oven is 1.3×10 5 pa. Example 4

[0052] The main technical scheme of this embodiment is basically the same as that of Embodiment 1. For features not explained in this embodiment, the explanation in Embodiment 1 is adopted and will not be repeated here. The difference between this embodiment and Embodiment 1 is that:

[0053] In step (i), clean and drain the aconite root and set aside for later use. Spread a layer of coarse salt on the bottom of the pickling container, then spread a layer of aconite root, and then spread a layer of coarse salt, and so on. After pickling, the undissolved coarse salt is recovered and reused. Pickle for 12 hours.

[0054] In step (ii), the aconite root is placed in water and steamed at a constant temperature for 8 hours, with the temperature controlled at 50°C; the aconite root is directly sliced ​​or peeled and then sliced.

[0055] In step (iii), soak the aconite slices in water for 2 hours each time, and then change the water; soak for a total of 3 times.

[0056] In step (iv), add koji and jujube juice to the soaked aconite tablets, and keep the mixture at a constant temperature of 25°C for 48 hours; wherein, 8g of koji and 250g of jujube juice are added per kilogram of aconite tablets, and the jujube juice is prepared by adding 2kg of water per kilogram of jujube, beating the jujube with pulp, and filtering the filtrate.

[0057] In step (V), the drying method is staged heating drying: the aconite tablets are placed in an oven, kept at 50°C for 30 minutes, heated to 80°C for 60 minutes, and heated to 110°C for 30 minutes; the air pressure in the oven is 1.2×10 5 pa. Example 5

[0058] The main technical solution of this embodiment is basically the same as that of Embodiment 4, except that:

[0059] In step (a), marinate for 48 hours;

[0060] In step (ii), the mixture is steamed at a constant temperature of 80° C. for 12 h.

[0061] In step (iii), each soaking and bleaching is performed for 3 hours, for a total of 2 soaking and bleaching times.

[0062] In step (iv), the temperature is kept constant at 25°C for 72 hours; wherein, 20g of distiller's yeast and 400g of jujube juice are prepared for each kilogram of aconite tablets, and the jujube juice is prepared by adding 3kg of water to each kilogram of jujube, beating the jujube, and filtering the filtrate to obtain the filtrate.

[0063] In step (V), the drying method is staged heating drying: drying at 80°C for 90 minutes, drying at 110°C for 120 minutes, and drying at 140°C for 90 minutes; the pressure in the oven is 1.5×10 5 pa. Example 6

[0064] The main technical scheme of this embodiment is basically the same as that of Embodiment 5, except that in step (iii), each immersion and bleaching is performed for 2.5 hours, for a total of 2 immersion and bleaching times.

[0065] Comparative test and test results

[0066] The present invention reduces the toxicity of Heishun Tablets mainly in two ways, the first is to use salt pickling to replace the bile solution, the second is to control the conversion of diester alkaloids into monoester alkaloids in an ethanol aqueous solution environment without excessive hydrolysis through a unique process, and the second way can improve the efficacy of Heishun Tablets. For the first way, it can be clearly known from the principle and actual operation that the metal ions brought by the bile solution are not introduced, the toxicity is low, and it can be known without testing and comparison. For the second way, the effects of different processing processes are known by comparing the diester alkaloids and monoester alkaloids in different processing processes.

[0067] (1) Test subjects

[0068] Test objects No. 1 to 3: the black tablets prepared in Examples 1 to 3;

[0069] Test object No. 4: The same raw material ratio and method as in Example 1 were used, except that pure water was used instead of distiller's yeast and jujube juice in step (4);

[0070] Test object No. 5: The same raw material ratio and method as in Example 1 were adopted, except that in step (4), koji was added but pure water was used instead of jujube juice;

[0071] Test object No. 6: The same raw material ratio and method as in Example 1 were adopted, but in step (4), only jujube juice was added instead of koji.

[0072] (2) Test of diester alkaloid and monoester alkaloid content

[0073] 2.1 Test Method

[0074] 2.1.1 Crush the test object into powder, sieve through a No. 3 sieve to take 2.00g, weigh 3 portions in parallel, place in a stoppered conical flask, add 2 mL of ammonia test solution (40% ammonia water by volume), add 50 mL of ether, weigh the mass, ultrasonicate for 30 minutes, make up the weight of the volatilization with ether, and filter. Take 25 mL of the filtrate, recover the solvent under reduced pressure below 40°C to dryness, add 3 mL of 0.05% hydrochloric acid and methanol mixed solution by volume to dissolve, filter with a 0.22μm filter membrane after the residue is completely dissolved, and take the filtrate, which is the test solution, for later use.

[0075] 2.1.2 Take 0.3g of each of the reference substances: benzoylmeaconitine (BMA), benzoylmeaconitine (BAC), benzoylhypaconitine (BHA), meaconitine (MA), aconitine (AC), and hypoaconitine (HA), add 0.05% by volume hydrochloric acid-methanol mixed solution to prepare a mixed reference substance mother solution and calculate the concentration.

[0076] 2.1.3 Take the test sample solution and the mixed reference solution of known concentration, and use chromatographic analysis to determine the contents of the six main alkaloids BMA, BAC, BHA, MA, AC, and HA in Heishun Tablets (the detected contents are converted into percentage contents after calculation); among them, the sum of the contents of benzoylmesaconitine (BMA), benzoylmesaconitine (BAC), and benzoylhypaconitine (BHA) is the diester alkaloid content, and the sum of the contents of meaconitine (MA), aconitine (AC), and hypoaconitine (HA) is the monoester alkaloid content.

[0077] 2.2 Test results of diester alkaloids and monoester alkaloids

[0078] Table 1 Alkaloid content test results

[0079]

[0080] Through testing, it can be concluded that the Heishun tablets (Examples 1 to 3 corresponding to No. 1 to 3) prepared by the processing process of the present invention have a lower content of diester alkaloids and a higher content of monoester alkaloids, that is, the Heishun tablets prepared by the processing process of the present invention are low in toxicity and high in efficiency.

[0081] By comparing No. 1 and No. 2, it can be concluded that the staged heating and drying method can be beneficial to the conversion of diester alkaloids into monoester alkaloids.

[0082] By comparing No. 1 and No. 3, it can be inferred that the use of micro-pressurization can be beneficial to the conversion of diester alkaloids into monoester alkaloids.

[0083] By comparing No. 1 and No. 4, it can be inferred that distiller's yeast and jujube juice can effectively promote the conversion of diester alkaloids into monoester alkaloids.

[0084] By comparing No. 1 and No. 5, and No. 4 and No. 5, it can be inferred that koji can promote the conversion of diester alkaloids into monoester alkaloids, but the effect is not as good as the effect of adding koji and jujube juice together.

[0085] By comparing No. 1 and No. 6, and No. 4 and No. 6, it can be inferred that simple jujube juice can hardly promote the conversion of diester alkaloids into monoester alkaloids.

[0086] (3) Observation of the appearance and taste of Heishun tablets

[0087] Table 2 Appearance observation and tongue tasting results of different processes

[0088]

[0089] It can be inferred from Table 2 that jujube juice can improve the appearance color and gloss of Heishun tablets.

[0090] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit the scope of protection of the claims. A person skilled in the art should understand and modify or replace the technical solutions of the present invention with equivalents by referring to the preferred embodiments, but the technical solutions of the present invention are substantially the same and within the scope of protection.

Claims

1. A method for preparing Heishunpian, characterized in that: The following steps are involved: (1) Wash and marinate: Wash the aconite root, drain the water, spread a layer of coarse salt on the bottom of the marinating container, then spread a layer of aconite root, and then spread a layer of coarse salt. Marinate for 12 to 48 hours until the aconite root becomes hard and salt crystals form on the surface; (ii) Steaming and slicing: Put the pickled aconite into water and steam it at a constant temperature for 8 to 12 hours at a temperature of 50 to 80°C, and then slice it; (III) Soaking: Soak the aconite tablets in water for 2 to 3 times, each time for 2 to 3 hours and change the water; (IV) Toxicity reduction and efficacy enhancement: add wine yeast and jujube juice to the soaked aconite tablets, with 8-20g of wine yeast and 250-400g of jujube juice per kilogram of aconite tablets, and treat at a constant temperature of 25-40°C for 48-72 hours. The jujube juice is prepared by pulping and filtering pitted jujubes and water in a ratio of 1 kg: 2-3 kg; (V) Segmented pressure drying: Place the aconite tablets in an oven and bake at 50-80°C for 30-90 minutes, then heat to 80-110°C for 60-120 minutes, and then heat to 110-140°C for 30-90 minutes. The pressure in the oven is 1.2×10 5 ~1.5×10 5 Pa.

2. The method for preparing Heishunpian according to claim 1, characterized in that: In step (ii), the aconite root can be sliced ​​directly or peeled and then sliced.

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