Processing method and quality control method of characteristic cinnamomum camphora core decoction pieces

Abstract

The invention belongs to the technical field of processing and quality control of traditional Chinese medicine decoction pieces, and mainly relates to a processing method and a quality control method of Cinnamomum camphora characteristic cortex cinnamomi decoction pieces. The method comprises the following steps: firstly, soaking a cortex cinnamomi medicinal material in water, then moistening, peeling, cutting salix leaves, and drying. According to the invention, parameterization of the processing method is realized, and a quality control method of the cortex cinnamomi decoction pieces is established, so that the cortex cinnamomi decoction pieces are more controllable, and reference and basis are provided for standardized application of cortex cinnamomi processing.

Description

Technical Field

[0001] The invention belongs to the technical field of preparation and quality control of Chinese herbal medicine slices, and particularly relates to a preparation method and a quality control method of Zhangbang characteristic cinnamon heart slices. Background Art

[0002] Cinnamon heart is the dried young branch of Cinnamomum cassia Presl, a plant of Lauraceae. It has the functions of sweating and relieving muscles, warming and unblocking meridians, assisting yang and transforming qi, balancing and descending qi, and is used for colds, cold pain in the abdomen, amenorrhea due to cold blood, joint pain, phlegm and fluid retention, edema, palpitations, and running pig. The detailed processing technology of cinnamon heart is not included in the 2020 edition of the "Chinese Pharmacopoeia" and various local standards; there are few records in ancient books. The "Complete Book of Chinese Herbal Medicine Processing of Camphor Tree" records: take thick branches and soak them in clean water for 24 to 36 hours, then wrap them in sacks for about 7 to 10 days (spray water once a day) until soft, peel them, cut them into willow leaves, and dry them in the sun. However, the above-mentioned process does not specify detailed process parameters, has poor operability, cannot adapt to the current market, and the corresponding quality control methods have not been reported, which seriously restricts the industrial development of cinnamon heart. Summary of the invention

[0003] The purpose of the present invention is to provide a processing method and quality control method for Zhangbang characteristic cinnamon heart decoction pieces, so as to solve the problems of the shortcomings of the existing recorded cinnamon heart processing technology and the lack of quality control method.

[0004] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:

[0005] The present invention provides a method for preparing Zhangbang characteristic cinnamon heart decoction pieces, comprising the following steps:

[0006] Step 1: Soak the cleaned cinnamon core medicinal material in water at 15-35°C for 24-36 hours, and then moisten it with water for 7-10 days (spraying water once a day) until the water absorption of the cinnamon core reaches 15-35%, thereby obtaining a moist cinnamon core;

[0007] Step 2: Slice the moistened cinnamon core to obtain sliced ​​cinnamon core;

[0008] Step 3: Dry the cut cinnamon core at 50-70° C. for 12-18 hours until the moisture content of the cinnamon core does not exceed 12.0%, and sieve out the debris to obtain cinnamon core slices;

[0009] Furthermore, in step 2, the slices are cut into oblique slices with a short diameter of 3 to 10 mm.

[0010] The present invention also provides a quality control method for Zhangbang specialty cinnamon heart decoction pieces, which includes the following detection items: properties, moisture, total ash, extract, and cinnamaldehyde content.

[0011] Further, it is characterized in that the cinnamon core is round or oval in shape, with a short diameter of 3 to 10 mm. The wood of the cut surface is yellowish white to yellowish brown, the pith is round or slightly square, and there is occasionally residual reddish brown to brown epidermis that has not been removed. It is hard and brittle, has a unique aroma, and tastes sweet and slightly spicy.

[0012] Furthermore, it is characterized in that the moisture content shall not exceed 13.0%, the total ash content shall not exceed 3.0%, and the extract shall not be less than 4.0% when measured by the alcohol-soluble extract hot soaking method using ethanol as the solvent.

[0013] Furthermore, it is characterized in that the cinnamaldehyde content is not less than 0.6%.

[0014] The present invention discloses a processing method and quality control method for cinnamon heart slices. The present invention realizes parameterization of the processing method and establishes a quality control method for cinnamon heart slices, including: properties, moisture, total ash, extract, and cinnamaldehyde content. The slice quality control method of the present invention fills the gap in the quality evaluation of cinnamon heart, makes the quality of cinnamon heart slices more controllable, and provides a reference and basis for the standardized application of cinnamon heart processing. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] In order to more clearly illustrate the specific implementation manner of the present invention or the technical solution in the prior art, the drawings used in the specific implementation manner or the description of the prior art will be briefly introduced below.

[0016] Figure 1 Guixin processing process flow chart

[0017] Figure 2 HPLC chromatograms of cinnamaldehyde reference substance and cinnamon heart slice test substance DETAILED DESCRIPTION

[0018] The following is a further detailed description of the preparation method and quality control method of the Zhangbang characteristic cinnamon heart decoction pieces of the present invention in conjunction with specific embodiments.

[0019] Embodiment 1: the research of moistening time of cinnamon heart slices

[0020] 1. Take 8kg of cinnamon heart medicinal materials, remove the attachments and impurities attached to the surface of the medicinal materials, pass through No. 2 sieve to remove impurities, and the impurity rate after cleaning is less than 2%;

[0021] 2. Divide the cleaned cinnamon heart medicinal materials into 4 portions, soak them in water at 25℃ for 24 hours, then put them into a medicine moistening machine, spray water once a day, and select four conditions of 7 days, 8 days, 9 days and 10 days for moistening, record the water absorption of the medicinal materials during moistening, take them out, peel them, cut them into willow leaves, and dry them at 60℃ for 16 hours.

[0022] 3. Determination of cinnamaldehyde content

[0023] Instrument: Waters alliance e2695 high performance liquid chromatograph, Empower chromatography workstation, PDA detector.

[0024] Chromatographic column: Shimadzu ODS-3C18 (250mm×4.6mm, 5μm)

[0025] Mobile phase: acetonitrile-water (32:68)

[0026] Detection wavelength: 290nm

[0027] Flow rate: 1.0ml / min

[0028] Column temperature: 30°C

[0029] The theoretical plate number calculated based on the cinnamaldehyde peak should not be less than 3000.

[0030] Preparation of reference solution: Take an appropriate amount of cinnamaldehyde reference substance, weigh it accurately, and add methanol to make a solution containing 10 μg per 1 ml.

[0031] Preparation of test solution: Take about 0.5 g of the powder of the product (passed through No. 4 sieve), weigh it accurately, place it in a stoppered conical flask, add 25 ml of methanol accurately, weigh it, treat it with ultrasound (power 250 W, frequency 40 kHz) for 30 minutes, let it cool, weigh it again, make up the lost weight with methanol, shake it well, filter it, accurately measure 1 ml of the filtrate, place it in a 25 ml volumetric flask, add methanol to the scale, shake it well, and obtain it.

[0032] Accurately pipette 10 μl of the reference solution and the test solution respectively, inject into the liquid chromatograph, and measure. The results are shown in Table 1.

[0033] Table 1 Research results of different moistening time

[0034]

[0035] Conclusion: According to the above table, the soaking time has no significant effect on the content of water, extract and cinnamaldehyde in cinnamon heart slices. Therefore, the soaking time of cinnamon heart is determined to be 7 to 10 days.

[0036] Example 2: Preparation of 5 batches of samples of cinnamon bark slices

[0037] Medicinal materials: The medicinal materials of Cassia cassia are collected from Yulin and Fangchenggang, Guangxi, and are authenticated as authentic by Chinese medicine masters.

[0038] Instruments and equipment: XY-500 continuous circulating water washing machine (Jinan Bochuang Pharmaceutical Equipment Co., Ltd.), CH-P1200 peeling machine (Jinan Bochuang Pharmaceutical Equipment Co., Ltd.), YQJ-300 multifunctional oblique slice machine (Shandong Aoge Machinery Equipment Co., Ltd.), SS-054 drying oven (Anguo Yaoxing Machinery Factory)

[0039] Take the cinnamon heart medicinal material, remove the attachments and impurities attached to the surface of the medicinal material, pass it through a No. 2 sieve to remove impurities, and the impurity rate after purification is less than 2%. Soak it in water at 25°C for 24 hours, then put it in a steaming place for 8 days, spray it with water once a day, take it out, peel it, cut it into willow leaves, and dry it at 60°C for 16 hours to prepare 5 batches of cinnamon heart medicinal slices.

[0040] Example 3: Establishment of a quality control method for cinnamon bark

[0041] 3.1 Properties

[0042] The five batches of samples collected this time are all oblique slices, all of which are round or oval slices with a short diameter of 3 to 10 mm. The wood of the cut surface is yellowish white to yellowish brown, the pith is round or slightly square, and there is occasionally some reddish brown to brown skin that has not been removed. It is hard and brittle, with a unique aroma and a sweet and slightly spicy taste.

[0043] 3.2 Moisture determination

[0044] The moisture content of 5 batches of cinnamon core was determined according to the fourth method of 0832 of the fourth part of the 2020 edition of the "Chinese Pharmacopoeia". The results are shown in Table 2.

[0045] Table 2 Moisture determination results

[0046]

[0047] Results: The average value of moisture content of 5 batches of samples was 7.30%. According to the General Rules for the Inspection of Medicinal Materials and Medicinal Slices in 0212 of the 2020 edition of the Chinese Pharmacopoeia, "Unless otherwise specified, the moisture content of medicinal materials shall not exceed 13%", the moisture limit is set as: "Not exceeding 13.0%".

[0048] 3.3 Determination of total ash

[0049] The total ash content of 5 batches of cinnamon bark slices was determined according to General Rules 2302 of Part IV of the 2020 edition of the Chinese Pharmacopoeia, and the results are shown in Table 3.

[0050] Table 3 Total ash content determination results

[0051]

[0052] Results: The average total ash content of 5 batches of samples was 1.14%. According to the National Drug Standard Work Manual and the actual test situation, the total ash content limit was set as: "not exceeding 3.0%".

[0053] 3.4 Leaching matter

[0054] The alcohol-soluble extract hot infusion method of the 2020 edition of the Chinese Pharmacopoeia was adopted, and ethanol was used as the solvent to determine the alcohol-soluble extracts of 5 batches of cinnamon bark slices. The results are shown in Table 4.

[0055] Table 4 Alcohol-soluble extract determination results

[0056]

[0057] Results: According to literature reports, the content of fat-soluble components such as cinnamaldehyde and cinnamic acid in the skin of cinnamon heart is generally 1 to 3 times higher than that in the wood. The processing process of cinnamon heart includes "peeling". Combined with the actual detection situation and reference literature reports, the limit of the extract was lowered by 20% on the basis of the detection mean. Finally, the limit of the extract of cinnamon heart decoction pieces was set as: "not less than 4.0%".

[0058] 3.5 Determination of cinnamaldehyde content

[0059] Cinnamon heart can induce sweating and relieve muscles, warm and unclog the meridians, assist yang and transform qi, and balance and descend qi. Among them, cinnamaldehyde, as the main component of cinnamon heart, has the effects of regulating body temperature and relieving pain.

[0060] Chromatographic conditions

[0061] Instrument: Waters alliance e2695 high performance liquid chromatograph, Empower chromatography workstation, PDA detector.

[0062] Chromatographic column: Shimadzu ODS-3C18 (250mm×4.6mm, 5μm)

[0063] Mobile phase: acetonitrile-water (32:68)

[0064] Detection wavelength: 290nm

[0065] Flow rate: 1.0ml / min

[0066] Column temperature: 30°C

[0067] The theoretical plate number calculated based on the cinnamaldehyde peak should not be less than 3000.

[0068] Preparation of reference solution: Take an appropriate amount of cinnamaldehyde reference substance, weigh it accurately, and add methanol to make a solution containing 10 μg per 1 ml.

[0069] Preparation of test solution: Take about 0.5 g of the powder of the product (passed through No. 4 sieve), weigh it accurately, place it in a stoppered conical flask, add 25 ml of methanol accurately, weigh it, treat it with ultrasound (power 250 W, frequency 40 kHz) for 30 minutes, let it cool, weigh it again, make up the lost weight with methanol, shake it well, filter it, accurately measure 1 ml of the filtrate, place it in a 25 ml volumetric flask, add methanol to the scale, shake it well, and obtain it.

[0070] Accurately pipette 10 μl of the reference solution and the test solution respectively, inject into the liquid chromatograph, and measure. The results are shown in Table 5. Figure 1 (A is cinnamaldehyde reference substance, B is cinnamaldehyde decoction piece test solution).

[0071] Table 5 Cinnamaldehyde determination results

[0072]

[0073] Results: According to literature reports, the content of cinnamaldehyde in the skin of cinnamon heart medicinal materials is generally 1 to 2 times higher than that in the wood. The processing technology of cinnamon heart includes "peeling". The average value of cinnamaldehyde content in cinnamon heart medicinal materials is 2.40%, and the average value of cinnamaldehyde content in cinnamon heart decoction pieces is 0.80%, and the average transfer rate is 33.34%. Therefore, combined with the actual detection situation and reference literature reports, the content limit was lowered by 20% on the basis of the detection mean value, and the final content limit of cinnamon heart was set as: "This product, calculated on the basis of dry product, contains not less than 0.6% cinnamaldehyde (C9H8O)".

[0074] The above description is only a preferred embodiment of the present invention and is not intended to limit the protection scope of the present invention. Therefore, any equivalent changes or modifications made in accordance with the patent scope of the present invention shall fall within the scope of the patent claims of the present invention.

Claims

1. A method for preparing Zhangbang specialty cinnamon heart slices, characterized in that: The steps include: Step 1: Soak the cleaned cinnamon core medicinal material in water at 15-35°C for 24-36 hours, and then moisten it with water for 7-10 days (spraying water once a day) until the water absorption of the cinnamon core reaches 15-35%, thereby obtaining a moist cinnamon core; Step 2: Slice the moistened cinnamon core to obtain sliced ​​cinnamon core; Step 3: Dry the cut cinnamon core at 50-70°C for 12-18 hours until the moisture content of the cinnamon core does not exceed 12.0%. Sieve out the debris to obtain the cinnamon core slices.

2. The method for preparing the Zhangbang specialty cinnamon heart slices according to claim 1, characterized in that: In step 2, the slices are oblique slices with a short diameter of 3 to 10 mm.

3. A quality control method for Zhangbang specialty cinnamon heart slices, characterized in that: The test items include: properties, moisture, total ash, extract, and cinnamaldehyde content.

4. The quality control method according to claim 3, characterized in that: The characteristics of the cinnamon core should be that this product is a sub-circular or oval piece with a short diameter of 3 to 10 mm. The wood of the cut surface is yellowish white to yellowish brown, the pith is sub-circular or slightly square, and there is occasionally residual reddish brown to brown skin that has not been removed. It is hard and brittle, has a unique aroma, and tastes sweet and slightly spicy.

5. The quality control method according to claim 3, characterized in that: The moisture content shall not exceed 13.0%, the total ash content shall not exceed 3.0%, and the extract shall not be less than 4.0% when measured by the alcohol-soluble extract hot soaking method using ethanol as the solvent.

6. The quality control method according to claim 3, characterized in that: The cinnamaldehyde content shall not be less than 0.6%.

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