Loquat syrup and preparation method thereof

Abstract

The invention discloses loquat syrup and a preparation method thereof, and relates to the field of medicines.The preparation method comprises the steps that folium eriobotryae, radix stemonae and platycodon grandiflorum are subjected to percolation extraction with an ethanol solution, and fat-soluble components in the three kinds of medicinal materials such as triterpenic acid components in the folium eriobotryae, alkaloid components in the radix stemonae and saponin components in the platycodon grandiflorum can be effectively extracted; meanwhile, medicine residues obtained after percolation, pericarpium papaveris, cynanchum glaucescens and cortex mori radicis are decocted and extracted together with water, water-soluble components such as alkaloids, flavonoids, polysaccharides and amino acids in the medicine residues can be effectively extracted, and the preparation method has the advantages of being easy to operate and implement, high in preparation efficiency, good in stability and the like; the quality and the clinical treatment effect of the loquat syrup can be obviously improved.

Description

Technical Field

[0001] The invention relates to the field of medicines, and in particular to loquat juice and a preparation method thereof. Background Art

[0002] Strong loquat dew nourishes yin and lungs, relieves cough and eliminates phlegm. It is used for bronchitis cough. The main ingredients include loquat leaves, poppy shells, stemona, radix scutellariae, mulberry bark, platycodon and menthol. At present, the main method of extracting active ingredients from raw materials is water decoction, and the effect of the product needs to be improved.

[0003] In view of this, the present invention is proposed. Summary of the invention

[0004] The object of the present invention is to provide loquat juice and a preparation method thereof.

[0005] The present invention is achieved in that:

[0006] In a first aspect, an embodiment of the present invention provides a method for preparing loquat juice, comprising:

[0007] Using a soaking solvent to soak loquat leaves, stemonae and platycodon grandiflorum; the soaking solvent includes ethanol;

[0008] The soaked product is subjected to percolation extraction with a percolation solvent to obtain a percolation liquid and a medicinal residue; the percolation solvent comprises ethanol;

[0009] The medicinal residues, poppy shell, white radix scutellariae, mulberry bark and water are mixed and boiled to obtain a decoction;

[0010] The percolate and the decoction are mixed.

[0011] In a second aspect, an embodiment of the present invention provides a loquat juice prepared by the preparation method described in the above embodiment.

[0012] The present invention has the following beneficial effects:

[0013] By analyzing the raw material components of loquat dew, percolation extraction of loquat leaves, Stemona japonica and Platycodon grandiflorum with ethanol solution can effectively extract the fat-soluble components in the three medicinal materials, such as triterpenoid acids in loquat leaves, alkaloids in Stemona japonica and saponins in Platycodon grandiflorum; at the same time, the percolation residues are boiled with poppy shell, white scutellaria and mulberry bark to effectively extract the water-soluble components such as alkaloids, flavonoids, polysaccharides and amino acids.

[0014] The preparation method provided by the embodiment of the present invention can fully extract the water-soluble components and fat-soluble components in the medicinal materials, has the advantages of simple operation, easy implementation, high preparation efficiency, good stability, etc., and can significantly improve the quality of the product and the clinical treatment effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for use in the embodiments are briefly introduced below. It should be understood that the following drawings only show certain embodiments of the present invention and therefore should not be regarded as limiting the scope. For ordinary technicians in this field, other related drawings can be obtained based on these drawings without creative work.

[0016] Figure 1 The invention provides a comparison of the results of the potassium bismuth iodide identification reaction of the stemona alkaloids carried out according to the pharmacopoeia standard and the strong loquat dew prepared by the present invention. DETAILED DESCRIPTION

[0017] In order to make the purpose, technical scheme and advantages of the embodiments of the present invention clearer, the technical scheme in the embodiments of the present invention will be described clearly and completely below. If the specific conditions are not specified in the embodiments, they are carried out according to conventional conditions or conditions recommended by the manufacturer. If the manufacturer of the reagents or instruments used is not specified, they are all conventional products that can be purchased commercially.

[0018] In view of the defects of the prior art, the embodiment of the present application provides a new method for preparing a strong loquat juice, which can effectively extract triterpenoid acids in loquat leaves, alkaloids in Stemona japonica, triterpenoid saponins in Platycodon grandiflorum and other poorly water-soluble components. It has been verified that the triterpenoid acids in loquat leaves can significantly reduce the number of coughs in rats, effectively inhibit the activity of inducible nitric oxide synthase (iNOS) in macrophages in the body, reduce the release of nitric oxide, and have a significant therapeutic effect on chronic bronchitis; the alkaloids contained in Stemona japonica can reduce bronchospasm caused by histamine, reduce the excitability of the respiratory center, inhibit the cough reflex, achieve the purpose of antitussive, and can treat cough, whooping cough, asthma and other symptoms; the expectorant effect of Platycodon grandiflorum is mainly caused by the triterpenoid saponins contained therein, which can stimulate the gastric mucosa in small doses, causing mild nausea, thereby reflexively increasing bronchial secretion. The preparation method provided in the embodiments of the present application can fully extract the water-soluble components and fat-soluble components in the above three medicinal materials at the same time, improve product quality and clinical treatment effect, and give full play to the therapeutic effect of each medicinal flavor in the prescription.

[0019] In one aspect, an embodiment of the present invention provides a method for preparing loquat juice, comprising:

[0020] Using a soaking solvent to soak loquat leaves, stemonae and platycodon grandiflorum; the soaking solvent includes ethanol;

[0021] The soaked product is subjected to percolation extraction with a percolation solvent to obtain a percolation liquid and a medicinal residue; the percolation solvent comprises ethanol;

[0022] The medicinal residues, poppy shell, white radix scutellariae, mulberry bark and water are mixed and boiled to obtain a decoction;

[0023] The percolate and the decoction are mixed.

[0024] In some embodiments, the loquat leaves, stemona and platycodon for soaking are loquat leaf powder, stemona powder and platycodon powder.

[0025] In some embodiments, the loquat leaf powder, the stemona powder and the platycodon powder are obtained by sieving loquat leaves, stemona and platycodon, respectively, and the sieve aperture used for sieving is 1 to 20 mm. The sieve aperture can be any one of 1, 2, 4, 6, 8, 10, 12, 14, 16, 18, 20 mm or a range between any two of them.

[0026] In some embodiments, the aperture of the sieve is 8-12 mm. The particle size of the medicinal material will affect the dissolution of the active ingredient during percolation. After crushing, passing through the 8-12 mm sieve will not affect the percolation speed and can improve the extraction efficiency of the soluble components.

[0027] In some embodiments, the loquat juice is strong loquat juice.

[0028] In some embodiments, the soaking solvent comprises: an ethanol solution with an ethanol volume fraction of 50% to 60%. The ethanol volume fraction can be any one of 50%, 52%, 54%, 55%, 56%, 58%, 60%, or a range between any two. Using ethanol percolation within a set concentration range can increase the transfer rate of triterpenoid acid components in loquat leaves, alkaloid components in Stemona tuberosa, and saponin components in Platycodon grandiflorum.

[0029] In some embodiments, the soaking time is ≥30 min. In other embodiments, the soaking time is ≥90 min;

[0030] In some embodiments, the soaking time is 90 to 200 minutes, specifically, it can be any one of 90, 100, 120, 140, 160, 180, 200 minutes or a range between any two of them.

[0031] In some embodiments, 160-200 L of soaking solvent is added for every 69 kg of loquat leaves. The volume of the soaking solvent added for every 69 kg of loquat leaves can be any one of 160, 170, 180, 190, 200 L or a range between any two thereof.

[0032] In some embodiments, the diafiltration solvent includes: an ethanol solution with an ethanol volume fraction of 50% to 60%; the ethanol volume fraction can be any one of 50%, 52%, 54%, 55%, 56%, 58%, 60% or a range between any two of them.

[0033] In some embodiments, the percolation flow rate of the percolation extraction is 2 to 4 ml / min·kg; the percolation flow rate can specifically be any one of 2, 2.5, 3, 3.5, 4 ml / min·kg or a range between any two of them.

[0034] In some embodiments, 340-380 L of the diafiltration solvent is used for diafiltration per 69 kg of loquat leaves. The 340-380 L can specifically be any one of 340, 350, 360, 370, 380 L or a range between any two of them.

[0035] Mixing the medicinal residue, poppy shell, white qian, mulberry bark and water and then decocting is conducive to extracting water-soluble effective components in each medicinal flavor, such as alkaloids, flavonoids, polysaccharides, amino acids, etc. In some embodiments, the decocting time is 1 to 3 hours, specifically any one of 1, 1.5, 2, 2.5, 3 hours or a range between any two of them.

[0036] In some embodiments, during decoction, 1600-2000 L of water is added for every 50 kg of poppy shell. The 1600-2000 L can specifically be any one of 1600, 1700, 1800, 1848, 1900, 2000 L or a range between any two of them.

[0037] In some embodiments, after decoction and before mixing with the percolate, the preparation method further comprises: concentrating the decoction;

[0038] In some embodiments, the concentration comprises: concentrating the decoction to a relative density of 1.20 to 1.22 at 40 to 60° C. The 40 to 60° C. may be any one of 40, 42, 44, 46, 48, 50, 52, 54, 56, 58, 60° C. or a range between any two thereof. The 1.20 to 1.22 may be any one of 1.2, 1.21, 1.22 or a range between any two thereof.

[0039] In some embodiments, the main ingredients of the loquat juice include, by weight: 65-75 parts of loquat leaves, 10-20 parts of stemonae, 1-12 parts of platycodon, 45-55 parts of poppy shells, 5-15 parts of radix scutellariae and 1-12 parts of mulberry bark.

[0040] In some embodiments, the preparation method further comprises: adding at least one of sodium benzoate, sucrose, menthol and essence to the product after the percolate and the decoction are mixed.

[0041] In some embodiments, after adding sodium benzoate and sucrose, the preparation method includes heating the product after adding sodium benzoate and sucrose, and then adding menthol and flavor after cooling.

[0042] Heating the product after adding sodium benzoate and sucrose can effectively reduce the microbial load in the liquid medicine and improve product safety. In some embodiments, the heating temperature is 80-120°C and the time is 10-60 minutes. The temperature can be any one of 80, 90, 100, 110, 120°C or a range between any two. The time can be any one of 10, 20, 30, 40, 50, 60 minutes or a range between any two.

[0043] In some embodiments, the main ingredients of the loquat juice include, by weight: 65-75 parts of loquat leaves, 10-20 parts of stemonae, 1-12 parts of platycodon, 45-55 parts of poppy shells, 5-15 parts of radix scutellariae, 1-12 parts of mulberry bark and 0.01-0.5 parts of menthol.

[0044] The weight portion of loquat leaf can be any one of 65, 66, 68, 69, 70, 72, 74, 75 parts or any two of the range. The weight portion of Stemona can be any one of 10, 12, 14, 15, 16, 18, 20 parts or any two of the range. The weight portion of Platycodon grandiflorum can be any one of 1, 2, 4, 6, 8, 10, 12 parts or any two of the range. The weight portion of Poppy shell can be any one of 45, 46, 48, 50, 52, 54, 55 parts or any two of the range. The weight portion of white scutellaria can be any one of 5, 6, 8, 9, 10, 12, 14, 15 parts or any two of the range. The weight portion of Morus alba can be any one of 1, 2, 4, 6, 8, 10, 12 parts or any two of the range. The weight portion of menthol can be specifically any one of 0.01, 0.05, 0.1, 0.15, 0.3, 0.5 or a range between any two of them.

[0045] The auxiliary materials of the loquat juice include: 1 to 5 parts of sodium benzoate, 580 to 620 parts of sweeteners and 0.05 to 0.4 parts of flavors.

[0046] The weight of sodium benzoate can be any one of 1, 2, 3, 4, and 5 parts, or any two of them. The weight of sweetener can be any one of 580, 590, 600, 610, and 620 parts, or any two of them. The weight of flavor can be any one of 0.05, 0.1, 0.15, 0.3, and 0.4 parts, or any two of them.

[0047] In some embodiments, before adding sodium benzoate, sucrose, menthol and flavors, the preparation method further comprises: allowing the product obtained by mixing the decoction and the percolation liquid to stand.

[0048] In some embodiments, the standing time is ≥ 10 to 24 hours; the 10 to 24 hours can be any one of 10, 11, 12, 13, 14, 16, 18, 20, 22, 24 hours or any two thereof. Sufficient standing can precipitate some insoluble precipitates, preferably standing for more than 12 hours.

[0049] In some embodiments, after the mixture of the decoction and the percolate is allowed to stand, the preparation method further comprises: taking the supernatant and concentrating it by centrifugation;

[0050] In some embodiments, the centrifugal concentration includes: removing the precipitate by centrifugation at a speed of 15000-25000 r / min, and concentrating the clarified liquid after centrifugation to a relative density of 1.05-1.10 at 40-60°C. The speed can be any one of 15000, 16000, 17000, 18000, 20000, 22000, 24000, 25000 r / min or a range between any two of them. The 40-60°C can be any one of 40, 42, 44, 46, 48, 50, 52, 54, 56, 58, 60°C or a range between any two of them. The 1.05-1.10 can be any one of 1.05, 1.06, 1.07, 1.08, 1.09, 1.10 or a range between any two of them. High-speed centrifugation within the set speed range can separate smaller insoluble particles suspended in the drug solution and improve the clarity of the drug solution.

[0051] In addition, an embodiment of the present invention further provides a loquat juice, which is prepared by the preparation method described in any of the above embodiments.

[0052] The features and performance of the present invention are further described in detail below in conjunction with the embodiments.

[0053] Example 1

[0054] A strong loquat juice and a preparation method thereof, comprising the following steps.

[0055] 1. Pretreatment: Take loquat leaf slices, stemonae slices and platycodon slices, and crush them into coarse powder through a 10mm pore size sieve using a powerful crusher.

[0056] 2. Percolation extraction: Take 69 kg of loquat leaf powder, 15 kg of Stemona crude powder and 6 kg of Platycodon crude powder after pretreatment, add 180 L of 55% ethanol aqueous solution with ethanol volume fraction for 2 hours, slowly add 360 L of 55% ethanol aqueous solution with ethanol volume fraction for percolation, percolate at a speed of 3 ml / min per kg, collect all the percolate and save it for later use.

[0057] 3. Decoction extraction: Take 50kg of poppy shell slices, 9kg of white scutellaria slices, and 6kg of mulberry bark slices, and decoct them together with the residues after percolation extraction. Add 1860L of drinking water and decoct for 2 hours, and filter the decoction.

[0058] 4. Concentration of decoction: The decoction filtrate is concentrated under reduced pressure to a relative density of 1.20 (60°C).

[0059] 5. Mix and let stand: Add all the percolate into the decoction concentrate, mix evenly and let stand for 12 hours.

[0060] 6. Centrifugal concentration: Take the supernatant after standing, and remove the precipitate by centrifugation at 20,000 r / min. After centrifugation, the liquid is concentrated under reduced pressure to a relative density of 1.05 (60°C).

[0061] 7. Preparation: Transfer the concentrate to a liquid preparation tank, add 2.5 kg of sodium benzoate and 600 kg of sucrose, heat to 100°C, maintain for 30 minutes, cool, add 1.2 kg of citric acid, 0.15 kg of menthol dissolved in 2000 ml of ethanol and 100 ml of banana essence while stirring, add water to 1000 L, stir and mix, and filter to obtain.

[0062] Example 2

[0063] A strong loquat juice and a preparation method thereof, comprising the following steps.

[0064] 1. Pretreatment: Take loquat leaf slices, stemonae slices and platycodon slices, and crush them into coarse powder through a 15mm pore size sieve using a powerful crusher.

[0065] 2. Percolation extraction: Take 69 kg of loquat leaf powder, 15 kg of Stemona crude powder and 6 kg of Platycodon crude powder after pretreatment, add 180 L of 55% ethanol aqueous solution with ethanol volume fraction for 2 hours, slowly add 360 L of 55% ethanol aqueous solution with ethanol volume fraction for percolation, percolate at a speed of 4 ml / min per kg, collect all the percolate and save it for later use.

[0066] 3. Decoction extraction: Take 50kg of poppy shell slices, 9kg of white scutellaria slices, and 6kg of mulberry bark slices, and decoct them together with the residues after percolation extraction. Add 1860L of drinking water and decoct for 2 hours, and filter the decoction.

[0067] 4. Concentration of decoction: The decoction filtrate is concentrated under reduced pressure to a relative density of 1.20 (60°C).

[0068] 5. Mix and let stand: Add all the percolate into the decoction concentrate, mix evenly and let stand for 12 hours.

[0069] 6. Centrifugal concentration: Take the supernatant after standing, and remove the precipitate by centrifugation at 20,000 r / min. After centrifugation, the liquid is concentrated under reduced pressure to a relative density of 1.05 (60°C).

[0070] 7. Preparation: Transfer the concentrate to a liquid preparation tank, add 2.5 kg of sodium benzoate and 600 kg of sucrose, heat to 100°C, maintain for 30 minutes, cool, add 1.2 kg of citric acid, 0.15 kg of menthol dissolved in 2000 ml of ethanol and 100 ml of banana essence while stirring, add water to 1000 L, stir and mix, and filter to obtain.

[0071] Example 3

[0072] A strong loquat juice and a preparation method thereof, comprising the following steps.

[0073] 1. Pretreatment: Take loquat leaf slices, stemonae slices and platycodon slices, and crush them into coarse powder through a 10mm pore size sieve using a powerful crusher.

[0074] 2. Percolation extraction: Take 69 kg of loquat leaf powder, 15 kg of Stemona crude powder and 6 kg of Platycodon crude powder after pretreatment, add 180 L of 55% ethanol aqueous solution with ethanol volume fraction for 2 hours, slowly add 360 L of 55% ethanol aqueous solution with ethanol volume fraction for percolation, percolate at a speed of 3 ml / min per kg, collect all the percolate and save it for later use.

[0075] 3. Decoction extraction: Take 50kg of poppy shell slices, 9kg of white scutellaria slices, and 6kg of mulberry bark slices, and decoct them twice with the residues after percolation extraction. Add 1240L of drinking water each time and decoct for 2 hours, and filter the decoction.

[0076] 4. Concentration of decoction: Combine the decoction filtrate and concentrate under reduced pressure to a relative density of 1.22 (60°C).

[0077] 5. Mix and let stand: Add all the percolate into the decoction concentrate, mix evenly and let stand for 12 hours.

[0078] 6. Centrifugal concentration: Take the supernatant after standing, and remove the precipitate by centrifugation at 20,000 r / min. After centrifugation, the liquid is concentrated under reduced pressure to a relative density of 1.05 (60°C).

[0079] 7. Preparation: Transfer the concentrate to a liquid preparation tank, add 2.5 kg of sodium benzoate and 600 kg of sucrose, heat to 100°C, maintain for 30 minutes, cool, add 1.2 kg of citric acid, 0.15 kg of menthol dissolved in 2000 ml of ethanol and 100 ml of banana essence while stirring, add water to 1000 L, stir and mix, and filter to obtain.

[0080] Example 4

[0081] A strong loquat juice and a preparation method thereof, comprising the following steps.

[0082] 1. Pretreatment: Take loquat leaf slices, stemonae slices and platycodon slices, and crush them into coarse powder through a 10mm pore size sieve using a powerful crusher.

[0083] 2. Percolation and concentration: 69 kg of loquat leaf powder, 15 kg of Stemona coarse powder and 6 kg of Platycodon coarse powder after pretreatment were added with 180 L of 55% ethanol aqueous solution for soaking for 2 hours, and then 360 L of 55% ethanol aqueous solution was slowly added for percolation at a rate of 3 ml / min per kg, and all the percolation liquid was collected. The percolation liquid was decompressed to recover ethanol and concentrated to a relative density of 1.05 (60° C.).

[0084] 3. Decoction and concentration: Take 50kg of poppy shell slices, 9kg of white scutellaria slices, and 6kg of mulberry bark slices, and decoct them together with the residues after percolation extraction. Add 1860L of drinking water and decoct for 2 hours, filter the decoction, and concentrate the filtrate under reduced pressure to a relative density of 1.05 (60°C).

[0085] 4. Mix and let stand: Mix the two concentrates and let stand for 12 hours.

[0086] 5. Centrifugation: Take the supernatant after standing and centrifuge at 20,000 r / min to remove the precipitate.

[0087] 6. Preparation: Transfer the concentrated liquid after centrifugation to a liquid preparation tank, add 2.5 kg of sodium benzoate and 600 kg of sucrose, heat to 100°C, keep for 30 minutes, cool, add 1.2 kg of citric acid, 0.15 kg of menthol dissolved in 2000 ml of ethanol and 100 ml of banana essence while stirring, add water to 1000 L, stir and mix, and filter to obtain.

[0088] Example 5

[0089] A strong loquat juice and a preparation method thereof, comprising the following steps.

[0090] 1. Pretreatment: Take loquat leaf slices, stemonae slices and platycodon slices, and crush them into coarse powder through a 15mm pore size sieve using a powerful crusher.

[0091] 2. Percolation extraction: Take 69 kg of loquat leaf powder, 15 kg of Stemona crude powder and 6 kg of Platycodon crude powder after pretreatment, add 180 L of 55% ethanol aqueous solution with ethanol volume fraction for 2 hours, slowly add 360 L of 55% ethanol aqueous solution with ethanol volume fraction for percolation, percolate at a speed of 4 ml / min per kg, collect all the percolate and save it for later use.

[0092] 3. Decoction extraction: Take 50kg of poppy shell slices, 9kg of white scutellaria slices, and 6kg of mulberry bark slices, and decoct them together with the residues after percolation extraction. Add 1860L of drinking water and decoct for 2 hours, and filter the decoction.

[0093] 4. Concentration of decoction: The decoction filtrate is concentrated under reduced pressure to a relative density of 1.20.

[0094] 5. Mix and let stand: Add all the percolate into the decoction concentrate, mix evenly and let stand for 12 hours.

[0095] 6. Concentration of supernatant: Take the supernatant after standing, recover ethanol under reduced pressure and concentrate to a relative density of 1.05.

[0096] 7. Preparation: Transfer the concentrate to a liquid preparation tank, add 2.5 kg of sodium benzoate and 600 kg of sucrose, heat to 100°C, maintain for 30 minutes, cool, add 1.2 kg of citric acid, 0.15 kg of menthol dissolved in 2000 ml of ethanol and 100 ml of banana essence while stirring, add water to 1000 L, stir and mix, and filter to obtain.

[0097] Positive control example

[0098] A strong loquat dew according to the 2020 edition of the Chinese Pharmacopoeia and a preparation method thereof, comprising the following steps.

[0099] 1. Decoction: Take 69kg of loquat leaves, 50kg of poppy shells, 15kg of Stemona, 9kg of Radix Phellodendri, 6kg of Morus alba, and 6kg of Platycodon grandiflorum and decoct twice, adding 1860L of water each time and decoct for 2 hours, combine the decoctions, filter, and concentrate the filtrate to a relative density of 1.05.

[0100] Add 2.5 g of sodium benzoate, stir to dissolve, add 600 g of sucrose, continue heating to boiling, keep for 20 minutes, let stand, filter, add appropriate amount of citric acid, appropriate amount of essence dissolved in ethanol and menthol, stir, mix well, let stand, filter, add water to 1000 ml, mix well, and you have it.

[0101] 2. Preparation: Transfer the concentrate to a liquid preparation tank, add 2.5 kg of sodium benzoate, stir to dissolve, add 600 kg of sucrose, continue to heat to boiling, keep for 20 minutes, let stand, filter, add 0.5 kg of citric acid, 0.15 kg of menthol dissolved in 2000 ml of ethanol and 100 ml of banana essence, stir, mix, let stand, filter, add water to 1000 L, mix, and you have it.

[0102] Test Example 1

[0103] Trait testing.

[0104] The strong loquat juice prepared according to the embodiments, comparative examples and positive control examples was compared with the properties of the strong loquat juice samples in each example, and the results are as follows.

[0105] Table 1 Character comparison results

[0106] Strong Loquat Dew Group Strong Loquat Dew Sample Batch Number Strong loquat juice sample properties Example 1 K2403001 Brown clear liquid, no precipitation Example 2 K2403002 Brown clear liquid, no precipitation Example 3 K2403003 Brown clear liquid, no precipitation Example 4 K2403004 Brown liquid with a small amount of precipitation Example 5 K2403005 Brown liquid with a small amount of precipitation Positive control example 2309061FR Brown liquid with a small amount of precipitation

[0107] Test Example 2

[0108] Water-soluble component detection.

[0109] According to the embodiments, comparative examples and positive control examples, strong loquat juice was prepared, and the morphine content in each strong loquat juice sample was compared. The determination method was the same as the method under the determination of the content of strong loquat juice in the Chinese Pharmacopoeia 2020 edition, and the results are as follows.

[0110] Table 2 Morphine content determination results

[0111]

[0112]

[0113] Test Example 3

[0114] Fat-soluble components detection.

[0115] Strong loquat juice was prepared according to the methods provided in the embodiments, comparative examples and positive control examples, and the contents of oleanolic acid and ursolic acid (derived from loquat leaves), alkaloid identification (derived from poppy shells and Stemona japonica), and platycodon saponin D content (derived from platycodon) in each strong loquat juice sample were compared.

[0116] (1) Oleanolic acid and ursolic acid content

[0117] method:

[0118] Chromatographic conditions and system suitability test: The chromatographic column is Sepax Aurethyst C18-H (250*4.6mm, 5μm); the column temperature is 30℃; the mobile phase is acetonitrile-methanol-0.5% ammonium acetate solution (67:12:21); the flow rate is 1ml / min; the detection wavelength is 210nm. The theoretical plate number calculated based on the ursolic acid peak should not be less than 5000.

[0119] Preparation of reference solution: Take appropriate amount of oleanolic acid reference substance and ursolic acid reference substance, weigh accurately, add ethanol to make a mixed solution containing 50 μg oleanolic acid and 0.2 mg ursolic acid per 1 ml.

[0120] Preparation of test solution: Accurately measure 20 ml of each strong loquat dew sample, extract it 4 times (15 ml, 15 ml, 15 m, 20 ml) with a mixed solution of n-butanol-methanol (10:1, water saturated) by strong shaking, combine the n-butanol-methanol (10:1, water saturated) solutions, wash with 15 ml of water saturated with n-butanol, discard the aqueous solution, take the n-butanol solution, evaporate it in a water bath, dissolve the residue in methanol and transfer it quantitatively to a 5 ml volumetric flask, dilute it to the scale with methanol, shake well, filter it with a microporous filter membrane (0.45 μm), and take the filtrate to obtain the test solution.

[0121] Determination method: Accurately pipette 10μl of reference solution and 10-20μl of test solution respectively, inject into liquid chromatograph, and determine. 30 H 48 O3) and ursolic acid (C 30 H 48 O3) total amount meter.

[0122] result:

[0123] Table 3 Oleanolic acid and ursolic acid content determination results

[0124]

[0125] (2) Stemona alkaloids

[0126] Method: Use identification reaction for comparison. Take 10 ml of each strong loquat dew sample, add sodium hydroxide test solution to make it alkaline, extract with 10 ml of chloroform, separate the lower layer solution, extract with 1% sulfuric acid solution, take the acid layer and add potassium bismuth iodide test solution, and compare the amount of orange-red precipitate generated by the two.

[0127] The results of the test are shown in Figure 1 From the amount of precipitation, it can be seen that the alkaloids in the strong loquat dew prepared by the present invention are significantly increased.

[0128] This identification reaction is dedicated to the identification of alkaloids. Before process optimization (positive control example), only a small amount of orange-red precipitate was generated in the sample, and this part of alkaloids mainly came from the water-soluble alkaloids extracted from poppy shells. After process optimization (example), more orange-red precipitates were produced, and the increase of this alkaloid mainly came from the fat-soluble alkaloids obtained by percolation extraction of Stemona, indicating that the content of alkaloids in the sample has been significantly improved after process optimization.

[0129] (3) Platycodon saponin D content

[0130] method:

[0131] Chromatographic conditions and system suitability test: octadecylsilane bonded silica gel as filler, YMC-Pack ODS-A chromatographic column (25cm*4.6mm, 5μm); column temperature 30°C; acetonitrile-water (25:75) as mobile phase, flow rate 1ml / min; detection by evaporative light scattering detector; the theoretical plate number calculated based on the platycodon saponin D peak should be no less than 3000.

[0132] Preparation of reference solution: Take an appropriate amount of Platycodon saponin D reference substance, weigh it accurately, and add methanol to make a solution containing 0.2 mg per 1 ml.

[0133] Preparation of test solution: Accurately measure 25 ml of each strong loquat dew sample, shake and extract 3 times with n-butanol saturated with water, 25 ml each time, combine the n-butanol solutions, wash with 50 ml of ammonia test solution, discard the ammonia solution, wash with 50 ml of water saturated with n-butanol, discard the water solution, recover the solvent with the n-butanol solution to dryness, add an appropriate amount of methanol to dissolve the residue, transfer to a 1 ml volumetric flask, add methanol to the scale, shake well, filter, and take the filtrate to obtain.

[0134] Determination method: Accurately pipette 10μl and 20μl of reference solution and 10-15μl of test solution respectively, inject into liquid chromatograph, determine, and calculate with external standard two-point method logarithmic equation to get the result.

[0135] result

[0136] Table 4 Platycodon saponin D content determination results

[0137]

[0138] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A method for preparing loquat juice, characterized in that: It includes: Using a soaking solvent to soak loquat leaves, stemonae and platycodon grandiflorum; the soaking solvent includes ethanol; The soaked product is subjected to percolation extraction with a percolation solvent to obtain a percolation liquid and a medicinal residue; the percolation solvent comprises ethanol; The medicinal residues, poppy shell, white radix scutellariae, mulberry bark and water are mixed and boiled to obtain a decoction; The percolate and the decoction are mixed.

2. The preparation method according to claim 1, characterized in that: The soaking solvent includes: an ethanol solution with an ethanol volume fraction of 50% to 60%; Optionally, the soaking time is ≥30 min; Optionally, the soaking time is ≥90 min; Optionally, the soaking time is 90 to 200 minutes; Optionally, for every 69 kg of loquat leaves, 160 to 200 L of soaking solvent is added; Optionally, the soaked loquat leaves, stemonae and platycodon grandiflorum are loquat leaf powder, stemonae powder and platycodon grandiflorum powder; Optionally, the loquat leaf powder, the stemona powder and the platycodon powder are obtained by sieving loquat leaves, stemona and platycodon, respectively, and the sieve used for sieving has an aperture of 1 to 20 mm.

3. The preparation method according to claim 1, characterized in that: The diafiltration solvent includes: an ethanol solution with an ethanol volume fraction of 50% to 60%; Optionally, the percolation flow rate of the percolation extraction is 2 to 4 ml / min·kg; Optionally, per 69 kg of loquat leaves, 340 to 380 L of the diafiltration solvent is used for diafiltration.

4. The preparation method according to claim 1, characterized in that: The decoction time is 1 to 3 hours; Optionally, during decoction, 1600-2000 L of water is added for every 50 kg of poppy shell.

5. The preparation method according to claim 1, characterized in that: After decoction and before mixing with the percolate, the preparation method further comprises: concentrating the decoction; Optionally, the concentration includes: concentrating the decoction to a relative density of 1.20 to 1.22 at 40 to 60°C.

6. The preparation method according to any one of claims 1 to 5, characterized in that: According to the weight percentage, the main ingredients of the loquat juice include: 65-75 parts of loquat leaves, 10-20 parts of stemonae, 1-12 parts of platycodon, 45-55 parts of poppy shells, 5-15 parts of radix scutellariae and 1-12 parts of mulberry bark.

7. The preparation method according to any one of claims 1 to 5, characterized in that: The preparation method further comprises: adding at least one of sodium benzoate, sucrose, menthol and essence to the product obtained by mixing the percolate and the decoction; Optionally, after adding sodium benzoate and sucrose, the preparation method comprises heating the product after adding sodium benzoate and sucrose, and then adding menthol and flavor after cooling; Optionally, the heating temperature is 80-120° C. and the heating time is 10-60 min.

8. The preparation method according to claim 7, characterized in that: According to the weight percentage, the main ingredients of the loquat juice include: 65-75 parts of loquat leaves, 10-20 parts of stemonae, 1-12 parts of platycodon, 45-55 parts of poppy shells, 5-15 parts of radix scutellariae, 1-12 parts of mulberry bark and 0.01-0.5 parts of menthol; The auxiliary materials of the loquat juice include: 1 to 5 parts of sodium benzoate, 580 to 620 parts of sweeteners and 0.05 to 0.4 parts of flavors.

9. The preparation method according to claim 7, characterized in that: Before adding sodium benzoate, sucrose, menthol and essence, the preparation method further comprises: allowing the mixture of the percolate and the decoction to stand; Optionally, the standing time is ≥10 to 24 hours; Optionally, after the mixture of the percolate and the decoction is allowed to stand, the preparation method further comprises: taking the supernatant and concentrating it by centrifugation; Optionally, the centrifugal concentration includes: removing the precipitate by centrifugation at a speed of 15000-25000 r / min, and concentrating the clarified drug solution after centrifugation to a relative density of 1.05-1.10 at 40-60°C.

10. A loquat juice, characterized in that: The compound is prepared by the preparation method according to any one of claims 1 to 9.

Images