CN115006479B - Areca flower oral liquid and preparation method thereof - Google Patents

Areca flower oral liquid and preparation method thereof Download PDF

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Publication number
CN115006479B
CN115006479B CN202210722372.XA CN202210722372A CN115006479B CN 115006479 B CN115006479 B CN 115006479B CN 202210722372 A CN202210722372 A CN 202210722372A CN 115006479 B CN115006479 B CN 115006479B
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betel nut
flower
oral liquid
enzymolysis
filtering
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CN115006479A (en
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赵坤
陈志平
王波超
郑维兵
胡俊武
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Hainan Jushen Pharmaceutical Co ltd
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Hainan Jushen Pharmaceutical Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/88Liliopsida (monocotyledons)
    • A61K36/889Arecaceae, Palmae or Palmaceae (Palm family), e.g. date or coconut palm or palmetto
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/46Ingredients of undetermined constitution or reaction products thereof, e.g. skin, bone, milk, cotton fibre, eggshell, oxgall or plant extracts
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/0087Galenical forms not covered by A61K9/02 - A61K9/7023
    • A61K9/0095Drinks; Beverages; Syrups; Compositions for reconstitution thereof, e.g. powders or tablets to be dispersed in a glass of water; Veterinary drenches
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P1/00Drugs for disorders of the alimentary tract or the digestive system
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P1/00Drugs for disorders of the alimentary tract or the digestive system
    • A61P1/14Prodigestives, e.g. acids, enzymes, appetite stimulants, antidyspeptics, tonics, antiflatulents
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P11/00Drugs for disorders of the respiratory system
    • A61P11/14Antitussive agents
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/10Preparation or pretreatment of starting material
    • A61K2236/19Preparation or pretreatment of starting material involving fermentation using yeast, bacteria or both; enzymatic treatment
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/333Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

Abstract

The invention provides an areca flower oral liquid and a preparation method thereof, wherein the areca flower oral liquid comprises the steps of taking areca flower medicinal materials, adding an ethanol solution containing sodium carbonate-sodium bicarbonate buffer solution for soaking and extracting twice, adopting two-section microwave compound enzymolysis and diluted enzymolysis to obtain an areca flower extract, concentrating, decolorizing with active carbon, filtering, concentrating into fluid extract, refrigerating, filtering, adding honey, filtering, filling and sterilizing to obtain the areca flower oral liquid. The betel flower oral liquid has good light transmittance, better clarity and glossiness, and alkaloid content of 0.161-0.175 mg.mL ‑1 The content of betel nut polyphenol is 0.400-0.426 mg.mL ‑1 The high temperature acceleration is carried out for 6 months, the loss rate of alkaloid content is 1.2-5.3%, the loss rate of betel nut polyphenol content is 2.4-8.5%, the appearance character of betel nut flower oral liquid is clear, the precipitation content is less, and the betel nut flower oral liquid has slightly sweet taste and slightly astringent taste, and eliminates the afterbitter taste. The invention has the advantages of simple production method, easy control of product quality, high treatment efficiency, environmental protection and no pollution.

Description

Areca flower oral liquid and preparation method thereof
Technical Field
The invention relates to the technical field of oral liquid preparation, in particular to betel nut flower oral liquid and a preparation method thereof.
Background
Areca catechu L is evergreen tree of Areca genus of Palmaceae, and Areca flower is male flower bud of Areca catechu, and has the advantages of multiple flowers, long flowering period, high yield, and multiple physiological active substances such as polyphenols, alkaloids, and microelements beneficial to human body, and has effects of invigorating stomach, quenching thirst, and relieving cough. In the prior art, betel nut flowers are used as raw materials for producing betel nut scented tea, betel nut flower wine, betel nut flower oral liquid and other products, and the betel nut flower wine has the effects of clearing heat from throat, moistening lung, promoting the production of body fluid to quench thirst and the like and is favored by consumers.
However, the existing method for improving the content of the alkaloids and the polyphenols in the betel nut flower oral liquid lacks, lacks the production of the mature betel nut flower oral liquid, and meanwhile, the alkaloids and the polyphenols in the betel nut are unstable and are easy to form complexes, so that the content of the active ingredients is reduced, the stability of the betel nut flower oral liquid is also reduced, the phenomena of flocculation turbidity and more precipitation generation of the product are easily caused, and the quality of the product is influenced.
Disclosure of Invention
In view of the above, the present invention aims to provide an areca flower oral liquid and a preparation method thereof, which solve the above problems.
The technical scheme of the invention is realized as follows:
a preparation method of betel flower oral liquid comprises the following steps:
s1, taking areca flower medicinal materials, adding ethanol solution with the volume concentration of 60-70% for soaking and extracting to obtain areca flower extracting solution; the ethanol solution with the volume concentration of 60-70% contains sodium carbonate-sodium bicarbonate buffer solution; the sodium carbonate-sodium bicarbonate buffer solution can provide a stable buffer environment for extracting betel nut flower medicinal materials, and improves the extraction efficiency;
s2, collecting betel nut extract, concentrating, adding activated carbon for decolorization, filtering while the extract is hot, concentrating into fluid extract, adding sodium benzoate, refrigerating at 4-10 ℃ for 22-26 hours, and filtering to obtain fluid extract filtrate;
s3, the mass volume ratio is 1g:4-5mL, adding water into honey, boiling, filtering, mixing the honey filtrate and the fluid extract filtrate, stirring, adding water to the formula amount, filtering, filling, and sterilizing to obtain the betel nut flower oral liquid.
Further, the immersion extraction comprises two extractions, wherein the first extraction is as follows: according to the mass ratio of the feed liquid of 1:6-8, adding ethanol solution with volume concentration of 60-70%, soaking and extracting for 45-50h, and filtering to obtain filtrate a and filter residue a; the second extraction is as follows: according to the mass ratio of the feed liquid of 1:5-7, adding 60-70% ethanol solution into the filter residue a, soaking and extracting for 20-30h, filtering to obtain filtrate b and filter residue b, and combining the filtrate a and the filtrate b to obtain betel nut flower extract.
Further, the first extraction is preceded by two-stage microwave composite enzymolysis, wherein cellulase is added into betel nut flowers, the microwave power is 500-600W, the first-stage microwave enzymolysis is carried out for 20-30min, the softening enzyme solution is added, and the second-stage microwave enzymolysis is carried out for 40-50min at the microwave power of 800-900W;
in the two-stage microwave composite enzymolysis, the addition amount of the cellulase is 0.2-0.3% of the weight of the betel nut flowers; in the two-stage microwave composite enzymolysis, the addition amount of the softening enzyme solution is 10-14% of the weight of the betel nut flowers.
Further, the second extraction is preceded by dilution and enzymolysis, and a softening enzyme solution is added into the filter residue a for enzymolysis for 40-50min; in the diluted enzymolysis, the addition amount of the softening enzyme solution is 20-24% of the weight of the filter residue a.
Further, the softening enzyme solution consists of the following components in mass ratio 1:0.05-0.07:0.2 of water, a softening enzyme and sodium carboxymethylcellulose; the sodium carboxymethyl cellulose has good fusion and dispersion effects, and can mutually permeate and mutually fuse with the softening enzyme in a static state, so that the suspension degree of the softening enzyme is improved, the enzymolysis effect of the softening enzyme is promoted, and meanwhile, when cellulase is adopted for enzymolysis firstly and then a softening enzyme solution is added, part of cellulase can also degrade sodium carboxymethyl cellulose, the system is prevented from being sticky, and the quality of a product is not influenced.
Further, the activity of the softening enzyme is 80-100U/g.
Further, the temperature of the first-stage enzymolysis is 50-60 ℃, and the temperature of the second-stage enzymolysis is 65-75 ℃; the specific enzymolysis temperature is favorable for improving the microwave effect, and meanwhile, the phenomenon that the raw materials are heated up locally too quickly can not be caused, so that the structure of the active ingredients is damaged.
Further, in step S1, the volume ratio of the ethanol solution to the sodium carbonate-sodium bicarbonate buffer solution is 1:0.02-0.04.
Further, in step S2, the betel nut extract is collected and concentrated to 20-30% of the original betel nut extract volume; the decolorizing temperature is 40-50deg.C, and decolorizing time is 10-15min; the relative density of the fluid extract is 1.05-1.12.
Further, each 1000mL of betel flower oral liquid contains 233g betel flower, 3.5g active carbon, 3g sodium benzoate and 100g honey.
Compared with the prior art, the invention has the beneficial effects that:
the invention adopts two-stage microwave compound enzymolysis and dilution enzymolysis to extract betel nut anther materials, controls parameters such as enzymolysis power, temperature, time and the like, combines a softening enzyme solution composed of specific activity softening enzyme and sodium carboxymethylcellulose, and correspondingly adjusts conditions such as extraction of impregnating solution, concentration, decoloration, refrigeration and the like, and the obtained betel nut flower oral liquid has good light transmittance, better clarity and glossiness and alkaloid content of 0.161-0.175 mg.mL -1 The content of betel nut polyphenol is 0.400-0.426 mg.mL -1 The content of the active ingredients is high, and the traditional Chinese medicine composition has better curative effects on relieving or treating listlessness, inappetence and cough with excessive phlegm; the high temperature accelerating experiment shows that the loss rate of alkaloid content is 1.2-5.3%, the loss rate of betel nut polyphenol content is 2.4-8.5%, the betel nut flower oral liquid has clear appearance, less sediment content, slightly sweet taste and slightly astringent taste, and the after-bitter taste is eliminated. The invention has the advantages of simple production method, easy control of product quality, high treatment efficiency, environmental protection and no pollution.
According to the invention, when the betel flower medicinal material is extracted by ethanol soaking, two sections of microwave compound enzymolysis and dilution enzymolysis are adopted to mutually cooperate, parameters such as enzymolysis power, temperature, time and the like are controlled, and a softening enzyme solution composed of specific activity softening enzyme and sodium carboxymethyl cellulose is combined, so that on one hand, the permeability of cell membranes is increased, the acceleration of outward diffusion of active ingredients is promoted, on the other hand, the electrostatic repulsive force among colloid particles can be increased, the electrostatic stability of colloidal particles is improved, the crosslinking effect of sodium carboxymethyl cellulose is promoted, the uniformity of a solution for subsequent dilution enzymolysis is also facilitated, the stability of an oral liquid is further improved, and the relative damage degree to alkaloids and betel polyphenol components is weakened; meanwhile, the diluted enzymolysis can further reduce the diameter of colloidal particles in the system, avoid the aggregation of colloidal particles and the reduction of the number of colloidal particles, improve the stability of the oral liquid, and the diluted enzymolysis is beneficial to avoiding the turbidity phenomenon caused by the softened enzyme, further improve the light transmittance of the oral liquid, and meanwhile, the specific softened enzyme activity can avoid increasing the complex formed between the active ingredients and reducing the content of alkaloid and betel nut polyphenol in the oral liquid; the two-stage microwave compound enzymolysis and the dilution enzymolysis are mutually cooperated, which is beneficial to improving the clarity and the stability of the oral liquid.
Detailed Description
In order to better understand the technical content of the present invention, the following provides specific examples to further illustrate the present invention.
The experimental methods used in the embodiment of the invention are conventional methods unless otherwise specified.
Materials, reagents, and the like used in the examples of the present invention are commercially available unless otherwise specified.
Example 1
An oral liquid of Arecae semen flower comprises Arecae semen flower 233g, active carbon 3.5g, sodium benzoate 3g and Mel 100g per 1000mL oral liquid of Arecae semen flower;
the preparation method of the oral liquid comprises the following steps:
s1, taking betel nut flower medicinal materials, adding ethanol solution with the volume concentration of 65% for soaking and extracting, wherein the soaking and extracting comprises two extractions, and the first extraction is as follows: according to the mass ratio of the feed liquid of 1:7, adding 65% ethanol solution by volume concentration, soaking and extracting for 48 hours, and filtering to obtain filtrate a and filter residue a; the second extraction is as follows: according to the mass ratio of the feed liquid of 1: adding 65% ethanol solution into the filter residue a, soaking and extracting for 24h, filtering to obtain filtrate b and filter residue b, and combining the filtrate a and the filtrate b to obtain betel nut flower extract;
the volume ratio is 1:0.02, adding sodium carbonate-sodium bicarbonate buffer solution into 65% ethanol solution by volume concentration;
the first extraction is preceded by two-stage microwave compound enzymolysis, wherein cellulase accounting for 0.2 percent of the weight of the areca flower is added into the areca flower, the microwave enzymolysis is carried out for 20min at 50 ℃ before the microwave power is 500W, the softening enzyme solution accounting for 10 percent of the weight of the areca flower is added, and the microwave enzymolysis is carried out for 40min at 65 ℃ after the microwave power is 800W;
the softening enzyme solution comprises the following components in percentage by mass: 0.06:0.2 of water, softened enzyme with activity of 90U/g and sodium carboxymethyl cellulose;
s2, concentrating the betel nut extract to 20-22% of the original betel nut extract volume, adding active carbon, decolorizing at 40-50deg.C for 10min, filtering while hot, concentrating to obtain fluid extract with relative density of 1.05-1.07, adding sodium benzoate, refrigerating at 4-10deg.C for 22 hr, and filtering to obtain fluid extract filtrate;
s3, the mass volume ratio is 1g:4mL, adding water into honey, boiling, filtering, mixing the honey filtrate and the fluid extract filtrate, stirring, adding water to the formula amount, filtering, filling, and sterilizing to obtain the betel nut flower oral liquid.
Example 2
An oral liquid of Arecae semen flower comprises Arecae semen flower 233g, active carbon 3.5g, sodium benzoate 3g and Mel 100g per 1000mL oral liquid of Arecae semen flower;
the preparation method of the oral liquid comprises the following steps:
s1, taking betel nut flower medicinal materials, adding ethanol solution with the volume concentration of 65% for soaking and extracting, wherein the soaking and extracting comprises two extractions, and the first extraction is as follows: according to the mass ratio of the feed liquid of 1:7, adding 65% ethanol solution by volume concentration, soaking and extracting for 48 hours, and filtering to obtain filtrate a and filter residue a; the second extraction is as follows: according to the mass ratio of the feed liquid of 1: adding 65% ethanol solution into the filter residue a, soaking and extracting for 24h, filtering to obtain filtrate b and filter residue b, and combining the filtrate a and the filtrate b to obtain betel nut flower extract;
the volume ratio is 1:0.04, adding sodium carbonate-sodium bicarbonate buffer solution into 65% ethanol solution by volume concentration;
the first extraction is preceded by two-stage microwave compound enzymolysis, wherein cellulase accounting for 0.3 percent of the weight of the areca flower is added into the areca flower, the microwave enzymolysis is carried out for 30min at 60 ℃ at the microwave power of 600W, the softening enzyme solution accounting for 14 percent of the weight of the areca flower is added, and the microwave enzymolysis is carried out for 50min at 75 ℃ at the microwave power of 900W;
the softening enzyme solution comprises the following components in percentage by mass: 0.06:0.2 of water, softened enzyme with activity of 90U/g and sodium carboxymethyl cellulose;
s2, concentrating the betel nut extract to 28-30% of the original betel nut extract volume, adding active carbon, decolorizing at 40-50deg.C for 15min, filtering while hot, concentrating to obtain fluid extract with relative density of 1.10-1.12, adding sodium benzoate, refrigerating at 4-10deg.C for 26 hr, and filtering to obtain fluid extract filtrate;
s3, the mass volume ratio is 1g:5mL, adding water into honey, boiling, filtering, mixing the honey filtrate and the fluid extract filtrate, stirring, adding water to the formula amount, filtering, filling, and sterilizing to obtain the betel nut flower oral liquid.
Example 3
An oral liquid of Arecae semen flower comprises Arecae semen flower 233g, active carbon 3.5g, sodium benzoate 3g and Mel 100g per 1000mL oral liquid of Arecae semen flower;
the preparation method of the oral liquid comprises the following steps:
s1, taking betel nut flower medicinal materials, adding ethanol solution with the volume concentration of 65% for soaking and extracting, wherein the soaking and extracting comprises two extractions, and the first extraction is as follows: according to the mass ratio of the feed liquid of 1:7, adding 65% ethanol solution by volume concentration, soaking and extracting for 48 hours, and filtering to obtain filtrate a and filter residue a; the second extraction is as follows: according to the mass ratio of the feed liquid of 1: adding 65% ethanol solution into the filter residue a, soaking and extracting for 24h, filtering to obtain filtrate b and filter residue b, and combining the filtrate a and the filtrate b to obtain betel nut flower extract;
the volume ratio is 1:0.03, adding sodium carbonate-sodium bicarbonate buffer solution into 65% ethanol solution;
the first extraction is preceded by two-stage microwave compound enzymolysis, wherein cellulase accounting for 0.2 percent of the weight of the areca flower is added into the areca flower, the microwave enzymolysis is carried out for 30min at 55 ℃ before the microwave power is 550W, then softening enzyme solution accounting for 12 percent of the weight of the areca flower is added, and the microwave enzymolysis is carried out for 50min at 70 ℃ after the microwave power is 850W;
the softening enzyme solution comprises the following components in percentage by mass: 0.06:0.2 of water, softened enzyme with activity of 90U/g and sodium carboxymethyl cellulose;
s2, concentrating the betel nut extract to 22-24% of the original betel nut extract volume, adding active carbon, decolorizing at 40-50deg.C for 12min, filtering while hot, concentrating to obtain fluid extract with relative density of 1.05-1.07, adding sodium benzoate, refrigerating at 4-10deg.C for 24 hr, and filtering to obtain fluid extract filtrate;
s3, the mass volume ratio is 1g:4mL, adding water into honey, boiling, filtering, mixing the honey filtrate and the fluid extract filtrate, stirring, adding water to the formula amount, filtering, filling, and sterilizing to obtain the betel nut flower oral liquid.
Example 4
The difference between this example and example 3 is that step S1 is further diluted and enzymatically hydrolyzed before the second extraction, and the specific steps are as follows:
s1, taking betel nut flower medicinal materials, adding ethanol solution with the volume concentration of 65% for soaking and extracting, wherein the soaking and extracting comprises two extractions, and the first extraction is as follows: according to the mass ratio of the feed liquid of 1:7, adding 65% ethanol solution by volume concentration, soaking and extracting for 48 hours, and filtering to obtain filtrate a and filter residue a; the second extraction is as follows: according to the mass ratio of the feed liquid of 1: adding 65% ethanol solution into the filter residue a, soaking and extracting for 24h, filtering to obtain filtrate b and filter residue b, and combining the filtrate a and the filtrate b to obtain betel nut flower extract;
the volume ratio is 1:0.03, adding sodium carbonate-sodium bicarbonate buffer solution into 65% ethanol solution;
the first extraction is preceded by two-stage microwave compound enzymolysis, wherein cellulase accounting for 0.2 percent of the weight of the areca flower is added into the areca flower, the microwave enzymolysis is carried out for 30min at 55 ℃ before the microwave power is 550W, then softening enzyme solution accounting for 12 percent of the weight of the areca flower is added, and the microwave enzymolysis is carried out for 50min at 70 ℃ after the microwave power is 850W;
the second extraction is preceded by dilution enzymolysis, 22% of softening enzyme solution by weight of the filter residue a is added into the filter residue a, and enzymolysis is carried out for 45min;
the softening enzyme solution comprises the following components in percentage by mass: 0.06:0.2 of water, softened enzyme with activity of 90U/g and sodium carboxymethyl cellulose;
s2, concentrating the betel nut extract to 22-24% of the original betel nut extract volume, adding active carbon, decolorizing at 40-50deg.C for 12min, filtering while hot, concentrating to obtain fluid extract with relative density of 1.05-1.07, adding sodium benzoate, refrigerating at 4-10deg.C for 24 hr, and filtering to obtain fluid extract filtrate;
s3, the mass volume ratio is 1g:4mL, adding water into honey, boiling, filtering, mixing the honey filtrate and the fluid extract filtrate, stirring, adding water to the formula amount, filtering, filling, and sterilizing to obtain the betel nut flower oral liquid.
Example 5
An oral liquid of Arecae semen flower comprises Arecae semen flower 233g, active carbon 3.5g, sodium benzoate 3g and Mel 100g per 1000mL oral liquid of Arecae semen flower;
the preparation method of the oral liquid comprises the following steps:
s1, taking betel nut flower medicinal materials, adding ethanol solution with the volume concentration of 65% for soaking and extracting, wherein the soaking and extracting comprises two extractions, and the first extraction is as follows: according to the mass ratio of the feed liquid of 1:7, adding 65% ethanol solution by volume concentration, soaking and extracting for 48 hours, and filtering to obtain filtrate a and filter residue a; the second extraction is as follows: according to the mass ratio of the feed liquid of 1: adding 65% ethanol solution into the filter residue a, soaking and extracting for 24h, filtering to obtain filtrate b and filter residue b, and combining the filtrate a and the filtrate b to obtain betel nut flower extract;
the volume ratio is 1:0.03, adding sodium carbonate-sodium bicarbonate buffer solution into 65% ethanol solution;
the first extraction is preceded by two-stage microwave compound enzymolysis, wherein cellulase accounting for 0.2 percent of the weight of the areca flower is added into the areca flower, the microwave enzymolysis is carried out for 30min at 55 ℃ before the microwave power is 550W, then softening enzyme solution accounting for 12 percent of the weight of the areca flower is added, and the microwave enzymolysis is carried out for 50min at 70 ℃ after the microwave power is 850W;
the second extraction is preceded by enzymolysis, wherein 12% of softening enzyme solution by weight of the filter residue a is added into the filter residue a, and the enzymolysis is carried out for 45min;
the softening enzyme solution comprises the following components in percentage by mass: 0.06:0.2 of water, softened enzyme with activity of 200U/g and sodium carboxymethyl cellulose;
s2, concentrating the betel nut extract to 22-24% of the original betel nut extract volume, adding active carbon, decolorizing at 40-50deg.C for 12min, filtering while hot, concentrating to obtain fluid extract with relative density of 1.05-1.07, adding sodium benzoate, refrigerating at 4-10deg.C for 24 hr, and filtering to obtain fluid extract filtrate; the method comprises the steps of carrying out a first treatment on the surface of the
S3, the mass volume ratio is 1g:4mL, adding water into honey, boiling, filtering, mixing the honey filtrate and the fluid extract filtrate, stirring, adding water to the formula amount, filtering, filling, and sterilizing to obtain the betel nut flower oral liquid.
Comparative example 1
The difference between this comparative example and example 4 is that the two-stage microwave complex enzymolysis and dilution enzymolysis are not performed in step S1, and the specific steps are as follows:
s1, taking betel nut flower medicinal materials, adding ethanol solution with the volume concentration of 65% for soaking and extracting, wherein the soaking and extracting comprises two extractions, and the first extraction is as follows: according to the mass ratio of the feed liquid of 1:7, adding 65% ethanol solution by volume concentration, soaking and extracting for 48 hours, and filtering to obtain filtrate a and filter residue a; the second extraction is as follows: according to the mass ratio of the feed liquid of 1: adding 65% ethanol solution into the filter residue a, soaking and extracting for 24h, filtering to obtain filtrate b and filter residue b, and combining the filtrate a and the filtrate b to obtain betel nut flower extract;
the volume ratio is 1:0.03, adding sodium carbonate-sodium bicarbonate buffer solution into 65% ethanol solution;
s2, concentrating the betel nut extract to 22-24% of the original betel nut extract volume, adding active carbon, decolorizing at 40-50deg.C for 12min, filtering while hot, concentrating to obtain fluid extract with relative density of 1.05-1.07, adding sodium benzoate, refrigerating at 4-10deg.C for 24 hr, and filtering to obtain fluid extract filtrate;
s3, the mass volume ratio is 1g:4mL, adding water into honey, boiling, filtering, mixing the honey filtrate and the fluid extract filtrate, stirring, adding water to the formula amount, filtering, filling, and sterilizing to obtain the betel nut flower oral liquid.
Comparative example 2
The difference between the comparative example and the example 4 is that the step S1 does not perform two-stage microwave composite enzymolysis, and the specific steps are as follows:
s1, taking betel nut flower medicinal materials, adding ethanol solution with the volume concentration of 65% for soaking and extracting, wherein the soaking and extracting comprises two extractions, and the first extraction is as follows: according to the mass ratio of the feed liquid of 1:7, adding 65% ethanol solution by volume concentration, soaking and extracting for 48 hours, and filtering to obtain filtrate a and filter residue a; the second extraction is as follows: according to the mass ratio of the feed liquid of 1: adding 65% ethanol solution into the filter residue a, soaking and extracting for 24h, filtering to obtain filtrate b and filter residue b, and combining the filtrate a and the filtrate b to obtain betel nut flower extract;
the volume ratio is 1:0.03, adding sodium carbonate-sodium bicarbonate buffer solution into 65% ethanol solution;
the second extraction is preceded by dilution enzymolysis, 22% of softening enzyme solution by weight of the filter residue a is added into the filter residue a, and enzymolysis is carried out for 45min;
the softening enzyme solution comprises the following components in percentage by mass: 0.06:0.2 of water, softening enzyme with activity of 80-100U/g and sodium carboxymethyl cellulose;
s2, concentrating the betel nut extract to 22-24% of the original betel nut extract volume, adding active carbon, decolorizing at 40-50deg.C for 12min, filtering while hot, concentrating to obtain fluid extract with relative density of 1.05-1.07, adding sodium benzoate, refrigerating at 4-10deg.C for 24 hr, and filtering to obtain fluid extract filtrate;
s3, the mass volume ratio is 1g:4mL, adding water into honey, boiling, filtering, mixing the honey filtrate and the fluid extract filtrate, stirring, adding water to the formula amount, filtering, filling, and sterilizing to obtain the betel nut flower oral liquid.
Test example 1
Determination of clarity: the transmittance of the betel flower oral liquid is measured by spectrophotometry, the higher the transmittance is, the higher the clarity is, the distilled water is used as blank, and the absorbance value is measured at 590-610 nm.
Determination of alkaloid content: taking 10mL of betel flower oral liquid, adding 80mL of diethyl ether, shaking uniformly, adding 4mL of ammonia reagent, shaking for 10min, adding 10g of anhydrous sodium sulfate, shaking for 10min, standing, separating and taking out diethyl ether, washing residues with diethyl ether for 3 times, 10mL each time, combining washing solutions of diethyl ether, adding 0.5g of talcum powder, shaking for 10min, standing, separating and taking out diethyl ether layer, washing water layer with a small amount of diethyl ether for 2 times, combining washing solutions of diethyl ether and diethyl ether layer, evaporating diethyl ether solution to about 20mL at low temperature, adding 20mL of 0.01M sulfuric acid titration solution, shaking for 10min, standingSeparating diethyl ether layer, extracting diethyl ether layer with water under shaking for 3 times (each time 5 mL), mixing the washing liquid and the acid solution, adding methyl red indicator 2-3 drops, titrating with 0.01M standard sodium hydroxide titration solution, and parallelly measuring for 3 times, wherein the alkaloid is ether-soluble alkaloid containing ether-soluble alkaloid with arecoline (C) 8 H 13 NO 2 ) And (5) counting.
Determination of betel nut polyphenol content: taking 10mL of betel flower oral liquid, adding 8mL of vanillin methanol solution with the concentration of 30g/L, shaking for 15min, adding 4mL of concentrated hydrochloric acid, shaking for 15min, carrying out water bath at 30 ℃ for 30min, measuring absorbance value at 500nm by adopting a spectrophotometry method, drawing a standard curve by using catechin standard substances, and carrying out parallel measurement for 3 times.
And (3) measuring the content of alkaloid and betel polyphenol of the prepared betel nut flower oral liquid, namely the content of alkaloid and betel nut polyphenol at the time of 0 month, placing the betel nut flower oral liquid in a constant temperature and constant humidity box, observing the stability test and the appearance property, measuring the content of alkaloid and betel nut polyphenol at the end of 6 months by measuring the temperature of the constant temperature and constant humidity box at 45+/-2 ℃ and the relative humidity of 65+/-5 percent, and observing the appearance property of the product.
The experimental results are shown in the following table:
as shown in the table, the betel flower oral liquid obtained by the invention has good light transmittance, better clarity and glossiness, and alkaloid content of 0.161-0.175 mg.mL -1 The content of betel nut polyphenol is 0.400-0.426 mg.mL -1 The high temperature accelerated experiment shows that the loss rate of alkaloid content is 1.2-5.3%, the loss rate of betel nut polyphenol content is 2.4-8.5%, betel nut flower oral liquid is clear, and the precipitation content is low. Example 4 compared with examples 1-3, the betel flower is subjected to dilution enzymolysis before the second ethanol extraction, which is helpful for improving the clarity and glossiness of the oral liquid, andthe loss rate of the content of the active ingredients is reduced, and the stability of the system is greatly improved; compared with example 5, the dilution enzymolysis is performed to help avoid turbidity caused by the softening enzyme, improve the light transmittance of the oral liquid, and increase the activity of the softening enzyme to promote the formation of a complex of active ingredients, thereby reducing the content of alkaloids and betel nut polyphenol.
Compared with comparative examples 1 and 2, the embodiment 4 has the advantages that through two-stage microwave composite enzymolysis, the microwave effect increases the permeability of cell membranes, promotes the outward diffusion of active ingredients, increases the electrostatic repulsive force between colloid particles, improves the electrostatic stability of colloidal particles, promotes the crosslinking action of sodium carboxymethyl cellulose, is beneficial to improving the uniformity of solution for subsequent dilution enzymolysis, further improves the stability of oral liquid, and reduces the relative damage degree to alkaloid and betel nut polyphenol components; meanwhile, the diameter of colloidal particles in the system can be further reduced by dilution enzymolysis, colloidal particle aggregation and reduction of the number of colloidal particles are avoided, and the two-section microwave compound enzymolysis and dilution enzymolysis are mutually cooperated, so that the clarity and stability of the oral liquid are improved.
Comparative example 3
The difference between the embodiment and the embodiment 4 is that the step S1 adopts two-section ultrasonic composite enzymolysis to replace two-section microwave composite enzymolysis, and the specific steps are as follows:
s1, taking betel nut flower medicinal materials, adding ethanol solution with the volume concentration of 65% for soaking and extracting, wherein the soaking and extracting comprises two extractions, and the first extraction is as follows: according to the mass ratio of the feed liquid of 1:7, adding 65% ethanol solution by volume concentration, soaking and extracting for 48 hours, and filtering to obtain filtrate a and filter residue a; the second extraction is as follows: according to the mass ratio of the feed liquid of 1: adding 65% ethanol solution into the filter residue a, soaking and extracting for 24h, filtering to obtain filtrate b and filter residue b, and combining the filtrate a and the filtrate b to obtain betel nut flower extract;
the volume ratio is 1:0.03, adding sodium carbonate-sodium bicarbonate buffer solution into 65% ethanol solution;
the first extraction is preceded by two-stage ultrasonic composite enzymolysis, wherein cellulase accounting for 0.2 percent of the weight of the areca flower is added into the areca flower, ultrasonic enzymolysis is carried out for 30min at 55 ℃ before ultrasonic power is 550W, softening enzyme solution accounting for 12 percent of the weight of the areca flower is added, and ultrasonic enzymolysis is carried out for 50min at 70 ℃ after ultrasonic power is 850W;
the second extraction is preceded by dilution enzymolysis, 22% of softening enzyme solution by weight of the filter residue a is added into the filter residue a, and enzymolysis is carried out for 45min;
the softening enzyme solution comprises the following components in percentage by mass: 0.06:0.2 of water, softened enzyme with activity of 90U/g and sodium carboxymethyl cellulose;
s2, concentrating the betel nut extract to 22-24% of the original betel nut extract volume, adding active carbon, decolorizing at 40-50deg.C for 12min, filtering while hot, concentrating to obtain fluid extract with relative density of 1.05-1.07, adding sodium benzoate, refrigerating at 4-10deg.C for 24 hr, and filtering to obtain fluid extract filtrate;
s3, the mass volume ratio is 1g:4mL, adding water into honey, boiling, filtering, mixing the honey filtrate and the fluid extract filtrate, stirring, adding water to the formula amount, filtering, filling, and sterilizing to obtain the betel nut flower oral liquid.
According to measurement, the transmittance of the betel flower is 58.2% when the betel flower is orally taken, and the leaching of protein, pectin and other components in the betel flower is easier to promote by ultrasound, so that the clarity of the oral liquid is affected by the ultrasound enzymolysis.
Test example 2
The experimental method comprises the following steps: 10 people are selected to form a sensory evaluation group to evaluate the taste of the betel nut flower oral liquid. Before evaluating the taste of the betel flower oral liquid, the betel flower oral liquid is fasted and water forbidden for at least 2 hours, each time, the betel flower oral liquid is subjected to sensory evaluation, 5mL of the betel flower oral liquid is contained in the mouth, the oral liquid is fully filled in the whole oral cavity, the betel flower oral liquid stays for at least 10 seconds, the taste after the betel flower oral liquid is noted to have bitter taste, the betel flower oral liquid needs to be gargled at least 3 times before and after each sensory evaluation, the sensory evaluation is totally divided into 10 minutes, and the evaluation score standard is as follows:
taste of Slightly sweet, slightly bitter and astringent Slightly sweet, slightly bitter and astringent Slightly sweet and slightly astringent Sweet
Score value 0 3 6 10
Sensory evaluation is carried out on the betel flower oral liquid according to the sensory evaluation standard, and the results are shown in the following table:
project Example 4 Comparative example 1
Score value 8 3
From the table, the sensory evaluation score of the betel nut oral liquid obtained in the embodiment 4 of the invention is 8 minutes, and the betel nut oral liquid has slightly sweet and astringent taste, which shows that the two-stage microwave compound enzymolysis and the diluted enzymolysis are performed, parameters such as enzymolysis power, temperature, time and the like are controlled, and the softening enzyme solution consisting of specific vitality softening enzyme and sodium carboxymethyl cellulose is combined, so that the after-bitter taste of the betel nut flower oral liquid can be eliminated to a certain extent, and the taste of the product and the compliance of patients, especially the compliance of children on medication can be improved.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.

Claims (6)

1. The preparation method of the betel nut flower oral liquid is characterized by comprising the following steps:
s1, taking areca flower medicinal materials, adding ethanol solution with the volume concentration of 60-70% for soaking and extracting to obtain areca flower extracting solution; the ethanol solution with the volume concentration of 60-70% contains sodium carbonate-sodium bicarbonate buffer solution;
the soaking extraction comprises two extractions, wherein the first extraction is as follows: according to the mass ratio of the feed liquid of 1:6-8, adding ethanol solution with volume concentration of 60-70%, soaking and extracting for 45-50h, and filtering to obtain filtrate a and filter residue a; the second extraction is as follows: according to the mass ratio of the feed liquid of 1:5-7, adding 60-70% ethanol solution into the filter residue a, soaking and extracting for 20-30h, filtering to obtain filtrate b and filter residue b, and combining the filtrate a and the filtrate b to obtain betel nut flower extract;
the first extraction is preceded by two-stage microwave compound enzymolysis, wherein cellulase is added into betel nut flowers, the microwave power is 500-600W, the first stage microwave enzymolysis is carried out for 20-30min, the softening enzyme solution is added, the microwave power is 800-900W, and the second stage microwave enzymolysis is carried out for 40-50min; in the two-stage microwave composite enzymolysis, the addition amount of the cellulase is 0.2-0.3% of the weight of the betel nut flowers; in the two-stage microwave composite enzymolysis, the addition amount of the softening enzyme solution is 10-14% of the weight of the betel nut flowers;
the second extraction is preceded by dilution and enzymolysis, and a softening enzyme solution is added into the filter residue a for enzymolysis for 40-50min; in the diluted enzymolysis, the addition amount of the softening enzyme solution is 20-24% of the weight of filter residue a;
the softening enzyme solution comprises the following components in percentage by mass: 0.05-0.07:0.2 of water, a softening enzyme and sodium carboxymethylcellulose;
s2, collecting betel nut extract, concentrating, adding activated carbon for decolorization, filtering while the extract is hot, concentrating into fluid extract, adding sodium benzoate, refrigerating at 4-10 ℃ for 22-26 hours, and filtering to obtain fluid extract filtrate;
s3, the mass volume ratio is 1g:4-5mL, adding water into honey, boiling, filtering, mixing the honey filtrate and the fluid extract filtrate, stirring, adding water to the formula amount, filtering, filling, and sterilizing to obtain the betel nut flower oral liquid.
2. The method for preparing betel nut flower oral liquid according to claim 1, wherein the activity of the softening enzyme is 80-100U/g.
3. The method for preparing betel nut flower oral liquid according to claim 1, wherein the temperature of the first stage enzymolysis is 50-60 ℃, and the temperature of the second stage enzymolysis is 65-75 ℃.
4. The method for preparing betel nut flower oral liquid according to claim 1, wherein in step S1, the volume ratio of the ethanol solution to the sodium carbonate-sodium bicarbonate buffer solution is 1:0.02-0.04.
5. The method for preparing betel nut flower oral liquid according to claim 1, wherein in step S2, betel nut extract is taken and concentrated to 20-30% of the original betel nut extract volume; the decolorizing temperature is 40-50deg.C, and decolorizing time is 10-15min; the relative density of the fluid extract is 1.05-1.12.
6. The method for preparing areca flower oral liquid according to claim 1, wherein each 1000mL of areca flower oral liquid contains 233g areca flower, 3.5g active carbon, 3g sodium benzoate and 100g honey.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1124586A (en) * 1994-01-07 1996-06-19 张坚 Betel palm flower oral liquid
CN102224932A (en) * 2011-06-15 2011-10-26 海南中盛合美生物制药有限公司 Areca flower extract and oral liquid

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1124586A (en) * 1994-01-07 1996-06-19 张坚 Betel palm flower oral liquid
CN102224932A (en) * 2011-06-15 2011-10-26 海南中盛合美生物制药有限公司 Areca flower extract and oral liquid

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