Preparation process and fingerprint spectrum of Xinan capsule

Abstract

The invention discloses a preparation process of a heart-'an capsule and a fingerprint spectrum of the heart-'an capsule, and relates to the technical field of traditional Chinese medicine preparation processes, the preparation process of the heart-'an capsule comprises extraction and preparation, the extraction comprises the following steps: a, extraction and concentration; b, drying; c, crushing; d, total mixing; e, bagging the totally mixed hawthorn leaf extract, and sealing for later use; the preparation method comprises the following steps: S1, preparing materials; s2, performing granulation; s3, drying; s4, granulating; s5, total mixing; s6, filling is carried out; s7, inner packaging; and S8, outer packaging, wherein specification packaging, boxing, boxing, packaging and warehousing are conducted. According to the invention, the hawthorn leaf coarse powder is subjected to reflux extraction through 50% ethanol, and is prepared into granules for filling the capsules, so that the production process is stable, and the contents of rhamnoside vitexin, glucoside vitexin, vitexin, rutin, hyperoside and chlorogenic acid in each batch of produced heart-'an capsules are stable, therefore, the heart-'an capsules produced by the production process are stable in quality, and the quality of the heart-'an capsules is greatly improved. The medicine effect of the product can be ensured, and the product quality is improved.

Description

Technical Field

[0001] This invention relates to the field of traditional Chinese medicine preparation technology, specifically to a preparation process and fingerprint spectrum of Xin'an Capsules. Background Technology

[0002] Xin'an Capsules are made from the ethanol extract of hawthorn leaves. Their main functions are to dilate coronary blood vessels, improve myocardial blood supply, and lower blood lipids. They are used to treat coronary heart disease, angina pectoris, chest tightness, palpitations, and hypertension. The production processes of Xin'an Capsules vary among different companies, resulting in some differences in the components of the capsules produced. Maintaining the stability of the content of each component in Xin'an Capsules is an important research direction for each company.

[0003] The existing manufacturing process for Xin'an capsules has the following defects:

[0004] Existing technology CN120939089A discloses a preparation process for improving the filling quality of Xin'an capsules. This technology includes six steps: weighing 4-5 kg ​​of hawthorn leaf extract powder and 0.5 kg of corn starch, then adding 95% ethanol, followed by soft material preparation, granulation, drying, pulverization, addition of excipients during total mixing, and filling. Excipients that improve the flowability of the powder are added to the pulverized powder. During mixing, the excipients cover the powder surface, forming a hydrophobic layer that directly blocks moisture contact, improving the flowability of the powder. This ensures that the filling weight deviates very little from the standard weight, thereby guaranteeing the safety of the finished capsules.

[0005] The above-mentioned technology produces Xin'an capsules by mixing hawthorn leaf extract powder with excipients. However, the stability of the content of various active ingredients in the produced Xin'an capsules cannot be guaranteed, and the content of active ingredients varies greatly among different Xin'an capsules, resulting in instability in efficacy. Therefore, a preparation process that can improve the stability of the content of various active ingredients in Xin'an capsules is needed to solve this problem. Summary of the Invention

[0006] One objective of this application is to provide a preparation process and fingerprint spectrum of Xin'an capsules, which can solve the technical problems raised in the prior art.

[0007] To achieve the above objectives, the present invention provides the following technical solution: a preparation process for Xin'an capsules, wherein the preparation process for Xin'an capsules includes extraction and formulation, and the extraction includes the following steps:

[0008] a. Extraction and concentration: Take hawthorn leaves, crush them into coarse powder, add 50% ethanol and reflux twice, filter, recover the ethanol from the filtrate and concentrate it into a thick paste.

[0009] b. Drying: Dry at a temperature below 60℃;

[0010] c. Pulverization: Pulverize the dried hawthorn leaf extract;

[0011] d. Blending: The hawthorn leaf extract was pulverized and blended for 30 minutes.

[0012] e. Pack the mixed hawthorn leaf extract into sealed bags for later use;

[0013] The formulation includes the following steps:

[0014] S1. Ingredients: Accurately weigh the materials according to the batch feeding amount;

[0015] S2. Granulation: Add the weighed hawthorn leaf extract, starch, and talc to a mixer and mix for 30 minutes to granulate.

[0016] S3. Drying: The drying temperature shall not exceed 60℃;

[0017] S4. Granulation: Dry granules are granulated using a 14-mesh sieve;

[0018] S5. Total Mixing: Place the dry granules into a mixer and mix for 30 minutes.

[0019] S6. Filling: Based on the particle content determination results, calculate the filling amount and use a capsule filling machine to fill the particles into empty capsules to obtain Xin'an capsules. Polish the Xin'an capsules.

[0020] S7. Inner packaging: The Xin'an capsules are packaged in aluminum-plastic packaging or bottles;

[0021] S8. Outsourcing: Packing instruction manuals, boxes, cartons, and warehouse storage.

[0022] Preferably, the batch feeding amount includes 330 kg of hawthorn leaf extract, 25 kg of starch and 145 kg of talc, and the batch feeding amount is granulated and packaged into 1 million empty capsules.

[0023] Preferably, the method for establishing the fingerprint spectrum of the Xin'an capsule is as follows: Take the granulated particles from step S2, then grind the particles into powder again, then add the powder to water to dissolve and obtain the Xin'an capsule solution, heat the Xin'an capsule solution to boiling, keep the Xin'an capsule solution boiling for 5 minutes, then let it cool naturally to room temperature, then filter the solution through a filter membrane, and inject the filtered solution into a liquid chromatograph for chromatographic determination to determine the content of six indicator components in the Xin'an capsule: vitexin rhamnoside, vitexin glucoside, vitexin, rutin, hyperoside and chlorogenic acid, and obtain the fingerprint spectrum of the Xin'an capsule.

[0024] Compared with the prior art, the beneficial effects of the present invention are:

[0025] 1. This invention uses 50% ethanol to reflux extract crude hawthorn leaf powder, which is then granulated and filled into capsules. The production process is stable, and the contents of vitexin rhamnoside, vitexin glucoside, vitexin, rutin, hyperoside, and chlorogenic acid in each batch of Xin'an capsules produced are stable. Therefore, the quality of Xin'an capsules produced by this process is stable, which can ensure the efficacy of the product, improve product quality, and make the content of each active ingredient in the product produced by the Xin'an capsule preparation process highly stable.

[0026] 2. The Xin'an Capsules produced by this invention have a high content of various active ingredients compared to other similar products, and the content of active ingredients in multiple batches of Xin'an Capsules is relatively consistent, resulting in high product quality stability and guaranteed efficacy. This ensures that the active ingredients in the Xin'an Capsules produced by the manufacturing process are at a high level, thus guaranteeing the drug's effectiveness.

[0027] 3. The Xin'an chromatogram produced by the process of this invention establishes the UPLC fingerprint spectrum of Xin'an capsules and performs similarity calculation. The similarity of multiple batches of products is consistent. Therefore, this process can ensure the stability and uniformity of the products. Attached Figure Description

[0028] Figure 1 This is a flowchart of the extraction process of the present invention;

[0029] Figure 2 This is a flowchart of the formulation process of the present invention;

[0030] Figure 3 A schematic diagram showing the vitexin rhamnoside content in the Xin'an capsules of various companies according to the present invention;

[0031] Figure 4 This is a schematic diagram showing the vitexin glucoside content in the Xin'an capsules of various companies according to the present invention.

[0032] Figure 5 This is a schematic diagram showing the rutin content in the Xin'an capsules of various companies according to the present invention;

[0033] Figure 6 This is a schematic diagram showing the hyperoside content in the Xin'an capsules of various companies according to the present invention;

[0034] Figure 7 This is a schematic diagram showing the vitexin content in the Xin'an capsules of various companies according to the present invention;

[0035] Figure 8 This is a schematic diagram showing the chlorogenic acid content in the Xin'an capsules of various companies according to the present invention;

[0036] Figure 9 The fingerprint spectrum of the Xin'an capsule of the present invention;

[0037] Figure 10This is a chromatographic fingerprint analysis report of traditional Chinese medicine according to the present invention;

[0038] Figure 11 This is a similarity analysis result diagram of the Xin'an Capsules produced by this invention. Detailed Implementation

[0039] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0040] Please see Figure 1 and Figure 2 The present invention provides an embodiment: a preparation process for a reassurance capsule;

[0041] The preparation process of Xin'an capsules includes extraction and formulation. The extraction process includes the following steps:

[0042] a. Extraction and concentration: Take hawthorn leaves, crush them into coarse powder, add 50% ethanol and reflux twice, filter, recover the ethanol from the filtrate and concentrate it into a thick paste.

[0043] b. Drying: Dry at a temperature below 60℃;

[0044] c. Pulverization: Pulverize the dried hawthorn leaf extract;

[0045] d. Blending: The hawthorn leaf extract was pulverized and blended for 30 minutes.

[0046] e. Pack the mixed hawthorn leaf extract into sealed bags for later use;

[0047] The formulation includes the following steps:

[0048] S1. Ingredients: Accurately weigh the materials according to the batch feeding amount;

[0049] S2. Granulation: Add the weighed hawthorn leaf extract, starch, and talc to a mixer and mix for 30 minutes to granulate.

[0050] S3. Drying: The drying temperature shall not exceed 60℃;

[0051] S4. Granulation: Dry granules are granulated using a 14-mesh sieve;

[0052] S5. Total Mixing: Place the dry granules into a mixer and mix for 30 minutes.

[0053] S6. Filling: Based on the particle content determination results, calculate the filling amount and use a capsule filling machine to fill the particles into empty capsules to obtain Xin'an capsules. Polish the Xin'an capsules.

[0054] S7. Inner packaging: The Xin'an capsules are packaged in aluminum-plastic packaging or bottles;

[0055] S8. Outsourcing: Packing instruction manuals, boxes, cartons, and warehouse storage.

[0056] The batch feed includes 330 kg of hawthorn leaf extract, 25 kg of starch and 145 kg of talc, and after granulation, the batch feed is packaged into 1 million empty capsules.

[0057] The fingerprint spectrum of Xin'an Capsules is established as follows: Take the granulated particles from step S2, grind the particles into powder again, add the powder to water to dissolve and obtain Xin'an Capsule solution, heat the Xin'an Capsule solution to boiling, keep boiling for 5 minutes, and then let it cool naturally to room temperature. Then filter the solution through a filter membrane, inject the filtered solution into a liquid chromatograph for chromatographic determination, determine the content of six index components in Xin'an Capsules: vitexin rhamnoside, vitexin glucoside, vitexin, rutin, hyperoside and chlorogenic acid, and obtain the fingerprint spectrum of Xin'an Capsules.

[0058] Please see Figure 1 and Figure 2 The present invention provides an embodiment: a preparation process for a reassurance capsule;

[0059] 1. Take hawthorn leaves, crush them into coarse powder, add 50% ethanol and reflux extract twice, filter, recover the ethanol from the filtrate and concentrate it into a thick paste.

[0060] 2. Dry at a temperature below 60℃;

[0061] 3. Crush the dried hawthorn leaf extract;

[0062] 4. Pulverize the hawthorn leaf extract and mix it with the whole mixture for 30 minutes.

[0063] 5. Pack the mixed hawthorn leaf extract into sealed bags for later use;

[0064] VI. Accurately weigh 330 kg of hawthorn leaf extract, 25 kg of starch, and 145 kg of talc powder according to the batch feeding amount;

[0065] 7. Weigh the hawthorn leaf extract, starch, and talc powder, add them to a mixer, mix for 30 minutes, granulate, take 4 granulated granules and grind them into powder, then add the powder to water to dissolve and obtain the Xin'an Capsule solution, heat the Xin'an Capsule solution to boiling, keep the Xin'an Capsule solution boiling for 5 minutes, then let it cool naturally to room temperature, then filter the solution through a filter membrane, inject the filtered solution into a liquid chromatograph for chromatographic determination, determine the content of 6 index components in Xin'an Capsule: vitexin rhamnoside, vitexin glucoside, vitexin, rutin, hyperoside and chlorogenic acid, and obtain the fingerprint spectrum of Xin'an Capsule;

[0066] 8. The drying temperature shall not exceed 60℃;

[0067] 9. Dry granules are sieved through a 14-mesh sieve;

[0068] 10. Place the dry granules into a mixer and mix for 30 minutes;

[0069] XI. Based on the particle content determination results, after calculating the filling amount, use a capsule filling machine to fill the particles into 1 million empty capsules to obtain Xin'an capsules, and then polish the Xin'an capsules.

[0070] 12. The Xin'an capsules shall be packaged in aluminum-plastic packaging or bottles;

[0071] Thirteen, pack the instruction manual, box, carton, and store in the warehouse.

[0072] Please see Figure 3 , Figure 4 , Figure 5 , Figure 6 , Figure 7 , Figure 8 , Figure 9 , Figure 10 and Figure 11 The present invention provides an embodiment;

[0073] Figure 3 The content of vitexin rhamnoside in Xin'an capsules produced by various companies is measured. Vitexin rhamnoside is an important component of total flavonoids in hawthorn leaves, which has the effects of dilating coronary blood vessels, improving myocardial blood supply, and lowering blood lipids. Vitexin rhamnoside has a concentration-dependent vasodilatory effect on isolated arterial rings and has a direct arterial dilation pharmacological effect. It can be used alone as a treatment drug for cardiovascular and cerebrovascular diseases. Therefore, this substance is used as one of the comparative control indicators for Xin'an capsules. Vitexin rhamnoside has a concentration-dependent vasodilatory effect on isolated arterial rings. The product produced by this invention has a relatively high content in the market, which will have a more significant effect on controlling myocardial blood supply and hyperlipidemia.

[0074] Figure 4The content of vitexin glucoside in Xin'an capsules produced by various companies was analyzed. Vitexin glucoside, a unique flavonoid component in hawthorn leaves, has shown significant antioxidant effects in in vitro experiments. As one of the main flavonoid components in hawthorn leaves, the analysis of the in vitro and in vivo experimental results of total flavonoids in hawthorn leaf extract preliminarily determined that vitexin glucoside plays a certain role in the treatment of hyperlipidemia, fatty liver, and protection of cardiac function by total flavonoid extract of hawthorn leaves.

[0075] Figure 5 This refers to the rutin content in the Xin'an capsules produced by various companies. Rutin is a vitamin that can reduce capillary permeability and fragility, maintain and restore the normal elasticity of capillaries, and is used to prevent and treat hypertension, cerebral hemorrhage, diabetic retinal hemorrhage, and hemorrhagic purpura. It can also be used to treat cardiovascular and cerebrovascular diseases, tumors, inflammation, etc.

[0076] Figure 6 The content of hyperoside in Xin'an capsules produced by various companies is listed. Hyperoside has multiple effects such as anti-tumor, anti-aging, anti-depression, and anti-inflammation. At the same time, it can also regulate the circulatory system, immune system, digestive system, and nervous system. Among its various pharmacological effects, its anti-oxidative stress damage and anti-apoptosis effects have always been a research hotspot.

[0077] Figure 7 This refers to the content of vitexin in the Xin'an capsules produced by various companies. Vitexin's main function is to promote blood circulation, remove blood stasis, regulate qi, and unblock the meridians. It is used for chest pain caused by blood stasis obstructing the meridians, with symptoms such as chest tightness, shortness of breath, stabbing pain in the precordial region, palpitations, forgetfulness, dizziness, and tinnitus. It is also used for symptoms such as angina pectoris, hyperlipidemia, and insufficient blood supply to the heart arteries. Recent studies have found that hawthorn and its leaves contain a compound called vitexin, which has anti-cancer effects.

[0078] Figure 8 This information pertains to the chlorogenic acid content in Xin'an capsules produced by various companies. Chlorogenic acid possesses pharmacological effects such as antibacterial, anti-inflammatory, detoxifying, choleretic, hypotensive, and leukocyte-increasing properties, as well as significantly increasing gastrointestinal motility and promoting gastric juice secretion. It exhibits strong inhibitory effects against Escherichia coli, Staphylococcus aureus, Streptococcus pneumoniae, and viruses. It also shows significant efficacy in treating acute pharyngitis and skin diseases. Clinically, it is used to treat acute bacterial infections and leukopenia caused by radiotherapy and chemotherapy. Years of clinical trials have confirmed that chlorogenic acid has a significant hypotensive effect with stable efficacy, no toxicity, and no side effects. Modern pharmacological experiments have demonstrated that chlorogenic acid has anticancer and cancer-suppressing effects. Japanese scholars have studied the mutagenicity-inhibiting effect of chlorogenic acid and found that this effect is related to antimutagenic components such as chlorogenic acid, revealing the important significance of chlorogenic acid in tumor prevention.

[0079] Based on the above tests and pharmacological analyses, it can be seen that the effective amounts of all active ingredients in the Xin'an Capsules produced by this invention can be well controlled. Except for hyperoside, due to slight differences in process control methods, the other ingredients are among the top in various manufacturers.

[0080] To better serve the market and ensure the uniformity, stability, reliability, and effectiveness of pharmaceutical products, the company is now conducting comprehensive analysis and testing of market products. Using the "2012 Edition of the Chromatographic Fingerprint Similarity Evaluation System for Traditional Chinese Medicine," a UPLC fingerprint of Xin'an Capsules has been established and similarity calculations performed to determine the product's uniformity and quality stability. Figure 9 , Figure 10 and Figure 11 It can be seen that the Xin'an Capsules produced by our company, batches 1902001, 1902002, 1903001 and 1903002, have the same similarity, while other manufacturers' batches are slightly different. Therefore, the existing process can guarantee the stability and uniformity of the product.

[0081] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the invention can be implemented in other specific forms without departing from its spirit or essential characteristics. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, all variations falling within the meaning and scope of equivalents of the claims are intended to be included within the present invention, and no reference numerals in the claims should be construed as limiting the rights involved.

Claims

1. A process for the preparation of heart care capsule, characterized by: The preparation process of the heart-peace capsule includes extraction and preparation, the extraction includes the following steps: a. extraction and concentration: take hawthorn leaves, crush into coarse powder, add 50% ethanol for reflux extraction twice, filter, recover ethanol from the filtered filtrate, and concentrate into thick paste; b. drying: dry below 60℃; c. crushing: crush the dried hawthorn leaf extract; d. total mixing: crush the hawthorn leaf extract for total mixing, total mixing time is 30 minutes; e. bag the hawthorn leaf extract after total mixing, seal, and reserve for use; The preparation includes the following steps: S1, batching: accurately weigh the materials according to the batch feeding amount; S2, granulation: put the weighed hawthorn leaf extract, starch, and talc into the mixer, mix for 30 minutes, and granulate; S3, drying: the drying temperature is not more than 60℃; S4, whole granulation: dry granules are whole granulated with 14 mesh sieve; S5, total mixing: put the dry granules into the mixer and mix for 30 minutes; S6, filling: according to the granule content determination results, calculate the loading amount, then use the capsule filling machine to fill the granules into the hollow capsules to obtain the heart-peace capsules, and polish the heart-peace capsules; S7, inner packaging: aluminum plastic package or bottle package the heart-peace capsules; S8, outer packaging: package the instructions, box, and case, and pack into the warehouse.

2. A process for the preparation of heart care capsule as claimed in claim 1 wherein: The batch feeding amount includes 330 kg of hawthorn leaf extract, 25 kg of starch, and 145 kg of talc, and the granulation after batch feeding is divided and packed in 1 million hollow capsules.

3. The fingerprint spectrum of the Xian capsule, which is suitable for the preparation process of the Xian capsule of claim 2, characterized in that: The method for establishing the fingerprint of the heart-peace capsule is as follows: take the granulation particles in step S2, then grind the particles into powder again, then dissolve the powder in water to obtain the heart-peace capsule solution, and heat and boil the heart-peace capsule solution, keep the heart-peace capsule solution boiling for 5 minutes, then naturally cool to room temperature, then filter the solution through a filter membrane, inject the filtered solution into a liquid chromatograph for chromatographic determination, determine the contents of the six index components in the heart-peace capsule, namely, vitexin rhamnoside, vitexin glucoside, vitexin, rutin, hyperoside, and chlorogenic acid, and obtain the fingerprint of the heart-peace capsule.

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