CN105166929B - Health drink beneficial to sleep as well as preparation method and detection method of health drink - Google Patents

Health drink beneficial to sleep as well as preparation method and detection method of health drink Download PDF

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CN105166929B
CN105166929B CN201510643602.3A CN201510643602A CN105166929B CN 105166929 B CN105166929 B CN 105166929B CN 201510643602 A CN201510643602 A CN 201510643602A CN 105166929 B CN105166929 B CN 105166929B
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health drink
solution
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health
preparation
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CN105166929A (en
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吕承洋
吕随民
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GANSU FUXINGHOU BIOLOGICAL MEDICAL TECHNOLOGY Co Ltd
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L2/00Non-alcoholic beverages; Dry compositions or concentrates therefor; Preparation or treatment thereof
    • A23L2/38Other non-alcoholic beverages
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N2030/022Column chromatography characterised by the kind of separation mechanism
    • G01N2030/027Liquid chromatography

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Abstract

The invention belongs to the technical field of food processing and particularly relates to a health drink beneficial to sleep as well as a preparation method and a detection method of the health drink. The health drink is prepared from raw materials in parts by weight as follows: 1-5 parts of Pilea pumila and 1-5 parts of flowers of Toona sinensis. The preparation method of the health drink comprises steps as follows: the Pilea pumila and the Toona sinensis are taken as per the weight ratio in a prescription, 5-15 times of water is added for decoction for 1-2 h, 5-10 times of water is added to decoction dregs for decoction for 0.5-1 h, water decoctions are mixed and filtered, a filtrate is concentrated and cooled, ethyl alcohol with the volume concentration of 95% is added until the concentration of the ethyl alcohol ranges from 60% to 75%, the mixture is stirred, then left to stand at the temperature of 4-8 DEG C for 12-48 h and filtered, the ethyl alcohol is recovered from a filtrate, a health tea extract solution is obtained, sucrose and water are added, sterilization is performed, and the health drink is prepared.

Description

A kind of health drink conducing to sleep and its preparation method and detection method
Technical field
The invention belongs to food processing technology field, it is related to a kind of health drink, specially one kind has promotion sleep work( The health drink of energy.
Background technology
Insomnia, i.e. sleep disorder.Show as difficulty falling asleep, intermittently discontinuous, and prematurely wake up, can not be again after waking up Continue to sleep, do not have enough sleep, malaise, burnout is felt, how because health condition is not good, pain, does not feel like oneself, circadian rhythm quilt Upset, sleep environment impact etc., also have fearness to sleep and have a sleepless night.
Insomnia is due to feelings will, diet internal injury, or after being ill and old, insufficiency of natural endowment, the cause of disease such as have a guilty consicence, and causes the mind Lose and support or confused and worried, thus leading to often to obtain the class illness that ortho is characterized.When being mainly shown as sleep Between the deficiency of depth and be unable to dispelling fatigue, regain one's strength and energy, the lighter's difficulty falling asleep, or sleep but not soundly, when when sleeping Wake up, or can not sleep again after waking up, heavy then be insomnia all night.
Insomnia is one of common clinical disease, though being not belonging to critical illness, hinders people's normal life, work, study And health, and can increase or induce the illnesss such as palpitaition, the obstruction of qi in the chest, dizziness, headache, apoplexy.Obstinate insomnia, brings to patient Long-term misery, or even form the dependence to sleeping medicine, and the sleeping medicine of long-term taking can cause iatrogenic disease.
Insomnia exists《Interior warp》In referred to as " insomnia ", " must not sleep ", " must not crouch ", and think that insomnia reason mainly has two Kind:One is other illnesss impact, and such as cough, vomiting, abdomen is full etc., must not make one reposal;Two is that negative and positive of qi and blood is become estranged, and making one can not Fall asleep.
In recent years, inventor adopts health drink of the present invention to be used for treatment insomnia, achieves preferable curative effect.
In the present invention:
Pilea mongolica is Urticaceae Pilea plant pilea mongolicaPilea pumila (L.) A. Cray [Urtica pumila L.; P. mongolica Wedd.]Herb or rhizome.
Ailanthus altissima flower is Meliaceae Chinese toon platymiscium Chinese toon Toona sinensis (A. Juss.) Roem. [Cedrela Sinensis A. Juss.] flower.
Content of the invention
It is an object of the invention to provide a kind of have the health drink promoting sleep function.
It is a further object of the present invention to provide the preparation method of this health drink.
The purpose of the present invention is achieved in the following ways:
A kind of have the health drink promoting sleep function, is made up of the raw material of following weight parts:Pilea mongolica 1~ 2 parts, 1~2 part of Ailanthus altissima flower.
Described health drink is preferably made up of the raw material of following weight parts:1 part of pilea mongolica, 1 part of Ailanthus altissima flower.
Described health drink is preferably made up of the raw material of following weight parts:1 part of pilea mongolica, 2 parts of Ailanthus altissima flower.
Described health drink is preferably made up of the raw material of following weight parts:2 parts of pilea mongolica, 1 part of Ailanthus altissima flower.
This health drink is made up of following methods:Take pilea mongolica, Ailanthus altissima flower by prescription weight proportion, plus 5~15 times Decocting boils 1~2 hour, and the dregs of a decoction add 5 again~and 10 times amount decoctings boil 0.5~1 hour, and decocting liquid merges, and filters, and filtrate concentrates, cold But, add the ethanol that volumetric concentration is 95% to be 60~75% to concentration of alcohol, be put in 4~8 DEG C after stirring and stand 12~48 hours, Filter, filtrate recycling ethanol, obtain health care tea extract, with sucrose, add water, sterilizing, make health drink.
This health drink is preferably made up of following methods:Take pilea mongolica, Ailanthus altissima flower by prescription weight proportion, plus 10 times Decocting boils 1.5 hours, and the dregs of a decoction add 6 times amount decoctings again and boil 1 hour, and decocting liquid merging twice is filtered, filtrate concentrates, cooling, added Volumetric concentration be 95% ethanol to concentration of alcohol be 70%, be put in after stirring 5 DEG C stand 24 hours, filter, filtrate recycling ethanol, Obtain health care tea extract, with sucrose, add water, sterilizing, make health drink.
This health drink carries out quality testing using following methods:
Using high effective liquid chromatography for measuring malvidin(malvidin)Content:
(1)Chromatographic condition:Chromatographic column is C18Chromatographic column;With ratio for 40~60:40~60 methyl alcohol -0.15% phosphoric acid is molten Liquid is mobile phase;Detection wavelength 300~330nm, 25~45 DEG C of column temperature;
(2)The preparation of reference substance solution:Precision weighs malvidin reference substance and is placed in volumetric flask, plus methyl alcohol dissolves and dilute Release to scale, shake up;Pipette above-mentioned solution and put volumetric flask, plus methanol constant volume, as reference substance stock solution;
(3)The preparation of need testing solution:Take health drink of the present invention, precision weighing, put in conical flask with cover, accurate addition Methyl alcohol, close plug, weighed weight, ultrasonically treated, let cool, more weighed weight, supply the weight of less loss with methyl alcohol, shake up, micropore is filtered Membrane filtration, takes subsequent filtrate, obtains final product need testing solution;
(4)Measure:Precision measures above-mentioned need testing solution, each 5~20 μ L of reference substance solution respectively, injects high-efficient liquid phase color Spectrometer, is detected.
This health drink preferably employs following methods and carries out quality testing:Using high effective liquid chromatography for measuring malvidin Content:
(1)Chromatographic condition:Chromatographic column is C18Chromatographic column;With ratio for 58:42 methyl alcohol -0.15% phosphoric acid solution is flowing Phase;Detection wavelength 328nm, 32 DEG C of column temperature;Number of theoretical plate is calculated by malvidin peak and should be not less than 3000;
(2)The preparation of reference substance solution:Precision weighs malvidin reference substance 10.00mg and is placed in 100mL volumetric flask, plus Methyl alcohol dissolves and is diluted to scale, shakes up;Pipette above-mentioned solution 10mL and put 25mL volumetric flask, plus methanol constant volume, as reference substance Stock solution;
(3)The preparation of need testing solution:Take health drink 10mL of the present invention, precision weighing, put in conical flask with cover, accurate Add methyl alcohol 10mL, close plug, weighed weight, ultrasonically treated 30min, let cool, more weighed weight, the weight of less loss is supplied with methyl alcohol Amount, shakes up, 0.45 μm of filtering with microporous membrane, takes subsequent filtrate, obtain final product need testing solution;
(4)Measure:Precision measures above-mentioned need testing solution, each 10 μ L of reference substance solution respectively, injects high performance liquid chromatography Instrument, is detected.
Described health drink can be used for preparing the health drink for the treatment of insomnia.
Experiment one:The experimental study of health drink treatment insomnia of the present invention
1 experiment material
Health drink of the present invention:Prescription:Pilea mongolica 5kg, Ailanthus altissima flower 5kg.Preparation method:Take stem by prescription weight proportion Pilea notata, Ailanthus altissima flower, plus 10 times of decoctings boil 1.5 hours, the dregs of a decoction add 6 times amount decoctings again and boil 1 hour, and decocting liquid merges twice, mistake Filter, filtrate concentrates, cooling, adds the ethanol that volumetric concentration is 95% to be 70% to concentration of alcohol, is put in 5 DEG C of standings 24 little after stirring When, filter, filtrate recycling ethanol, obtain health care tea extract of the present invention.
Contrast health drink A:Prescription:Pilea mongolica 10kg.Preparation method:Take pilea mongolica by prescription weight, plus 10 times Decocting boils 1.5 hours, and the dregs of a decoction add 6 times amount decoctings again and boil 1 hour, and decocting liquid merging twice is filtered, filtrate concentrates, cooling, added Volumetric concentration be 95% ethanol to concentration of alcohol be 70%, be put in after stirring 5 DEG C stand 24 hours, filter, filtrate recycling ethanol, Obtain contrasting health drink A extract.
Contrast health drink B:Prescription:Ailanthus altissima flower 10kg.Preparation method:Take Ailanthus altissima flower by prescription weight proportion, plus 10 times of decoctings Boil 1.5 hours, the dregs of a decoction add 6 times amount decoctings again and boil 1 hour, decocting liquid merging twice is filtered, filtrate concentrates, cooling, added volume Concentration be 95% ethanol to concentration of alcohol be 70%, be put in after stirring 5 DEG C stand 24 hours, filter, filtrate recycling ethanol, obtain Contrast health drink B extract.
Yellow Jackets:Beijing land for growing field crops Feng Tuo chemical technology Co., Ltd produces;
Strychnine nitrate parenteral solution:Beijing Double-Crane Pharmaceutical Co., Ltd produces;
Diazepam:Tianjin KingYork Amino Acid Co., Ltd. produces;
Animal:Kunming mouse, body weight 18g~22g, female dual-purpose, provided by Gansu university of TCM experimental center.
2 experimental techniques and result
The research of 2.1 pairs of spontaneous activity in mice
Mouse 60, male and female are regardless of, and are randomly divided into five groups, i.e. saline control group, contrast health drink A group, contrast Health drink B group, health drink group of the present invention, stable positive controls, every group 12.
Before administration, mouse is put into after adapting to 5 minutes in animal activity case, record animal walking time and the forelimb of 2 minutes The numerical value praising number of times upwards is as normal value.
Then give respectively:
Contrast health drink A group:Gavage gives contrast health drink A extract, and given low is 0.5mL/10g;
Contrast health drink B group:Gavage gives contrast health drink B extract, and given low is 0.5mL/10g;
Health drink group of the present invention:To health drink extract of the present invention, given low is 0.5mL/10g to gavage;
Stable positive controls give 0.01mg/10g and stabilize, gavage;
Saline control group gives same volume physiological saline, gavage.
Each group mouse, in latter 60 minutes of administration, measures mouse walking time by the same method and double forelimb praises number of times upwards.Knot Fruit with± s represents, the results are shown in Table 1-1.
The impact to spontaneous activity in mice number of times for the table 1-1(± s, n=12)
Note:Compare with physiological saline group, * P<0.05, * * P< 0.01;
In table, result shows:Health drink of the present invention all has obvious sedation to mouse, compares with physiological saline group There were significant differences(P< 0.01).Health drink group sedation of the present invention substantially, compares indifference with stable group(P> 0.05). Result shows:Health drink of the present invention has obvious sedation.
2.2 researchs on mice sleep impact
2.2.1 the impact to the mouse yellow Jackets length of one's sleep
Mouse 60, is randomly divided into 5 groups, i.e. saline control group, contrast health drink A group, contrast health drink B Group, health drink group of the present invention, stable positive controls, every group 12.
Contrast health drink A group:Gavage gives contrast health drink A extract, and given low is 0.5mL/10g;
Contrast health drink B group:Gavage gives contrast health drink B extract, and given low is 0.5mL/10g;
Health drink group of the present invention:To health drink extract of the present invention, given low is 0.5mL/10g to gavage;
Stable positive controls give 0.01mg/10g and stabilize, gavage;
Saline control group gives same volume physiological saline, gavage.
After gastric infusion 60 minutes, every group of mouse gives yellow Jackets 40mg/kg, lumbar injection respectively.Record mouse The length of one's sleep(With righting reflex loss as time for falling asleep, from righting reflex loss to recovery time for sleep time). The results are shown in Table 1-2.
The impact to the mouse yellow Jackets length of one's sleep for the table 1-2(± s, n=12)
2.2.2 the impact to mouse yellow Jackets sub-threshold dose
Mouse 60, is randomly divided into 5 groups, i.e. saline control group, contrast health drink A group, contrast health drink B Group, health drink group of the present invention, stable positive controls, every group 12.
Contrast health drink A group:Gavage gives contrast health drink A extract, and given low is 0.5mL/10g;
Contrast health drink B group:Gavage gives contrast health drink B extract, and given low is 0.5mL/10g;
Health drink group of the present invention:To health drink extract of the present invention, given low is 0.5mL/10g to gavage;
Stable positive controls give 0.01mg/10g and stabilize, gavage;
Saline control group gives same volume physiological saline, gavage.
After administration 30 minutes, each group mouse gives yellow Jackets 30mg/kg, lumbar injection respectively, observes and is recorded into Sleep number of animals(In 15 minutes, mouse righting reflex loss reaches mouse number on 1 minute as sleep number of animals), calculate sleep rate.Knot Fruit is shown in Table 1-3.
The impact to mouse pentobarbital sodium sub-threshold lull dosage for the table 1-3
Above two experiments all illustrate that health drink of the present invention and yellow Jackets have synergy, and health care of the present invention is described Beverage plays the role of hypnosis.
The research of 2.3 anti-strychnine nitrate convulsive attack effects
Mouse 60, male and female are regardless of, and are randomly divided into 5 groups, i.e. saline control group, contrast health drink A group, contrast Health drink B group, health drink group of the present invention, stable positive controls, every group 12.
Contrast health drink A group:Gavage gives contrast health drink A extract, and given low is 0.5mL/10g;
Contrast health drink B group:Gavage gives contrast health drink B extract, and given low is 0.5mL/10g;
Health drink group of the present invention:To health drink extract of the present invention, given low is 0.5mL/10g to gavage;
Stable positive controls give 0.01mg/10g and stabilize, gavage;
Saline control group gives same volume physiological saline, gavage.
Each group mouse, after administration 60 minutes, gives strychnine nitrate parenteral solution 1.5mg/kg, hypodermic injection, note respectively Record mice convulsion number(With mouse, generalized tonic occurs to faint from fear as index).The results are shown in Table 1-4.
The effect of table 1-4 anti-strychnine nitrate convulsive attack(n= 12)
Note:Compare with physiological saline group:**P < 0.01;
Result shows, stable group and health drink group of the present invention all play the role of to resist strychnine nitrate convulsive attack, with Physiological saline group compares, and is statistically analyzed the equal significance of difference.The anticonvulsant action of health drink of the present invention is strong, curative effect Good, illustrate that health drink of the present invention has anticonvulsant effect.
3 conclusions
The study find that, health drink of the present invention can suppress spontaneous activity in mice;Impact to mice sleep and penta bar ratio Appropriate sodium has synergy;Play the role of to resist strychnine nitrate convulsive attack.Illustrate health drink of the present invention have obvious calm, Hypnosis, anticonvulsant action, have the prospect of exploitation medicament for treating insomnia or health products.
Particularly, the action effect of health drink of the present invention is substantially better than contrast health drink A and contrast health drink B, Illustrate that in health drink of the present invention, compatibility between two kinds of flavour of a drug is superior, indispensable, the combination between two kinds of flavour of a drug creates Significantly synergistic function, creates the technique effect that one-plus-one is more than two.
Experiment two:The quality standard research of health drink of the present invention
Using malvidin content in high effective liquid chromatography for measuring health drink of the present invention
The preparation of 1 sample solution
The preparation of 1.1 reference substance solution
Precision weighs malvidin reference substance 10.00mg and is placed in 100mL volumetric flask, plus methyl alcohol dissolves and is diluted to quarter Degree, shakes up.Pipette above-mentioned solution 10mL and put 25mL volumetric flask, plus methanol constant volume, as reference substance stock solution(Malvidin 40.80μg/mL).
The preparation of 1.2 need testing solutions
Prescription:Pilea mongolica 5kg, Ailanthus altissima flower 5kg.
Preparation method:Take pilea mongolica, Ailanthus altissima flower by prescription weight proportion, plus 10 times of decoctings boil 1.5 hours, the dregs of a decoction add 6 again Times amount decocting boils 1 hour, and decocting liquid merging twice is filtered, filtrate concentrates, cooling, adds the ethanol that volumetric concentration is 95% to second Determining alcohol is 70%, is put in 5 DEG C and stands 24 hours, filter, filtrate recycling ethanol, obtain health care tea extract after stirring, plus in right amount Sucrose, add water, sterilizing, make health drink 20L.
Take health drink 10mL of the present invention, precision weighing, put in conical flask with cover, accurate addition methyl alcohol 10mL, close plug, claim Determine weight, ultrasonically treated 30min, let cool, more weighed weight, supply the weight of less loss with methyl alcohol, shake up, 0.45 μm of miillpore filter Filter, take subsequent filtrate, obtain final product need testing solution.
The preparation of 1.3 negative controls
Remaining composition taking in prescription composition in addition to pilea mongolica makes the negative controls without pilea mongolica, presses " 1.2 " are obtained negative control solution.Go out peak position in malvidin and absworption peak do not occur, illustrate in health drink of the present invention its He does not interfere with to the assay of malvidin composition.
2 chromatographic conditions
Chromatographic column is SHIMADZU C18Chromatographic column(5 μm, 4.6mm × 150.0mm, Shimadzu Corporation);With methyl alcohol -0.15% phosphorus Acid solution(58:42)For mobile phase;Detection wavelength 328nm, 32 DEG C of column temperature.Number of theoretical plate is calculated and should be not less than by malvidin peak 3000;With this understanding, in health drink of the present invention, malvidin separates well.
3 methodological studies.
3.1 the range of linearity
Accurate draw above-mentioned malvidin reference substance solution, plus methanol dilution become malvidin concentration to be respectively 0.816, 1.632nd, the solution of 3.264,4.896,6.528,8.160 μ g/mL, sample introduction 10 μ l successively.With peak area(Y)For ordinate, with Sample introduction concentration(X)Carry out linear regression for abscissa, obtain regression equation:
Y=3.638 × 104X 1.068 × 104, correlation coefficient r=0.9996.Show malvidin concentration 0.816~ With chromatographic peak area in good linear relation in the range of 8.160 μ g/mL.
3.2 precision test
Take the malvidin reference substance solution 10 μ l METHOD FOR CONTINUOUS DETERMINATION that concentration is 4.890 μ g/mL 5 times, RSD is 0.15%, shows Instrument precision is good.
3.3 stability test
Take same need testing solution 0,2,4,6,8h sample introduction 10 μ l respectively, record peak area, result shows:Test sample is molten Liquid is placed in 8h in room temperature and is stablized, and malvidin peak area RSD is 1.60%.
3.4 replica test
By health drink of the present invention, parallel extraction prepares 6 parts of need testing solutions, and sample introduction measures respectively, and RSD is 1.23%(n= 6), show that the method repeatability is good.
3.5 average recovery tests
Precision weighs each 9 parts of the health drink of the present invention of known content, adds the malvidin reference substance of respective amount, by confession The preparation method of test sample solution processes and measures.Average recovery result of the test is shown in Table 2-1.Malvidin average recovery rate is 97.7%, RSD are 1.66%, show that the method is accurate, reliable.
Table 2-1 recovery test result(n=9)
3.6 sample sizes measure.Take 4 batches, health drink sample of the present invention, according to the method for need testing solution preparation, 0.45 μ Sample introduction after m filtering with microporous membrane, different lot number health drink content of the present invention is shown in Table 2-2.
Table 2-2 sample determination result(n=3)
Experimental example three:Model case
Lee tries to gain, man, 61 years old, retired worker, because cerebrovascular disease goes into hospital before 3 months, because stress is big, causes mistake Sleep, after discharge, insomnia is not healed, and through multi-treatment, effect is bad, have palpitation, shortness of breath, palpitaition, dizziness, check and find that tongue is red, the heart Rule is uneven, One's spirits are drooping depressed, confirms as slightly having a sleepless night.
Drink health drink of the present invention, drink 1000mL daily, fraction is drunk, and continuously drinks 7 days, insomnia is cured, and has no Any bad reaction.
Specific embodiment
Embodiment 1:
Prescription:Pilea mongolica 5kg, Ailanthus altissima flower 5kg.
Preparation method:Take pilea mongolica, Ailanthus altissima flower by prescription weight proportion, plus 10 times of decoctings boil 1.5 hours, the dregs of a decoction add 6 again Times amount decocting boils 1 hour, and decocting liquid merging twice is filtered, filtrate concentrates, cooling, adds the ethanol that volumetric concentration is 95% to second Determining alcohol is 70%, is put in 5 DEG C and stands 24 hours, filter, filtrate recycling ethanol, obtain health care tea extract after stirring, plus in right amount Sucrose, add water, sterilizing, make health drink 20L.
Detection method:Using high effective liquid chromatography for measuring malvidin content:
(1)Chromatographic condition:Chromatographic column is SHIMADZU C18Chromatographic column;With ratio for 58:42 methyl alcohol -0.15% phosphoric acid is molten Liquid is mobile phase;Detection wavelength 328nm, 32 DEG C of column temperature;Number of theoretical plate is calculated by malvidin peak and should be not less than 3000;
(2)The preparation of reference substance solution:Precision weighs malvidin reference substance 10.00mg and is placed in 100mL volumetric flask, plus Methyl alcohol dissolves and is diluted to scale, shakes up;Pipette above-mentioned solution 10mL and put 25mL volumetric flask, plus methanol constant volume, as reference substance Stock solution;
(3)The preparation of need testing solution:Take health drink 10mL of the present invention, precision weighing, put in conical flask with cover, accurate Add methyl alcohol 10mL, close plug, weighed weight, ultrasonically treated 30min, let cool, more weighed weight, the weight of less loss is supplied with methyl alcohol Amount, shakes up, 0.45 μm of filtering with microporous membrane, takes subsequent filtrate, obtain final product need testing solution;
(4)Measure:Precision measures above-mentioned need testing solution, each 10 μ L of reference substance solution respectively, injects high performance liquid chromatography Instrument, is detected;
(5)Result:In every 10mL health drink of the present invention, malvidin content is 55.25 μ g.
Embodiment 2:
Prescription:Pilea mongolica 6.6kg, Ailanthus altissima flower 3.3kg.
Preparation method:Take pilea mongolica, Ailanthus altissima flower by prescription weight proportion, plus 10 times of decoctings boil 1.5 hours, the dregs of a decoction add 6 again Times amount decocting boils 1 hour, and decocting liquid merging twice is filtered, filtrate concentrates, cooling, adds the ethanol that volumetric concentration is 95% to second Determining alcohol is 70%, is put in 5 DEG C and stands 24 hours, filter, filtrate recycling ethanol, obtain health care tea extract after stirring, plus in right amount Sucrose, add water, sterilizing, make health drink 20L.
Detection method:Using high effective liquid chromatography for measuring malvidin content:
(1)Chromatographic condition:Chromatographic column is SHIMADZU C18Chromatographic column;With ratio for 58:42 methyl alcohol -0.15% phosphoric acid is molten Liquid is mobile phase;Detection wavelength 328nm, 32 DEG C of column temperature;Number of theoretical plate is calculated by malvidin peak and should be not less than 3000;
(2)The preparation of reference substance solution:Precision weighs malvidin reference substance 10.00mg and is placed in 100mL volumetric flask, plus Methyl alcohol dissolves and is diluted to scale, shakes up;Pipette above-mentioned solution 10mL and put 25mL volumetric flask, plus methanol constant volume, as reference substance Stock solution;
(3)The preparation of need testing solution:Take health drink 10mL of the present invention, precision weighing, put in conical flask with cover, accurate Add methyl alcohol 10mL, close plug, weighed weight, ultrasonically treated 30min, let cool, more weighed weight, the weight of less loss is supplied with methyl alcohol Amount, shakes up, 0.45 μm of filtering with microporous membrane, takes subsequent filtrate, obtain final product need testing solution;
(4)Measure:Precision measures above-mentioned need testing solution, each 10 μ L of reference substance solution respectively, injects high performance liquid chromatography Instrument, is detected;
(5)Result:In every 10mL health drink of the present invention, malvidin content is 33.54 μ g.
Embodiment 3:
Prescription:Pilea mongolica 3.3kg, Ailanthus altissima flower 6.6kg.
Preparation method:Take pilea mongolica, Ailanthus altissima flower by prescription weight proportion, plus 10 times of decoctings boil 1.5 hours, the dregs of a decoction add 6 again Times amount decocting boils 1 hour, and decocting liquid merging twice is filtered, filtrate concentrates, cooling, adds the ethanol that volumetric concentration is 95% to second Determining alcohol is 70%, is put in 5 DEG C and stands 24 hours, filter, filtrate recycling ethanol, obtain health care tea extract after stirring, plus in right amount Sucrose, add water, sterilizing, make health drink 20L.
Detection method:Using high effective liquid chromatography for measuring malvidin content:
(1)Chromatographic condition:Chromatographic column is SHIMADZU C18Chromatographic column;With ratio for 58:42 methyl alcohol -0.15% phosphoric acid is molten Liquid is mobile phase;Detection wavelength 328nm, 32 DEG C of column temperature;Number of theoretical plate is calculated by malvidin peak and should be not less than 3000;
(2)The preparation of reference substance solution:Precision weighs malvidin reference substance 10.00mg and is placed in 100mL volumetric flask, plus Methyl alcohol dissolves and is diluted to scale, shakes up;Pipette above-mentioned solution 10mL and put 25mL volumetric flask, plus methanol constant volume, as reference substance Stock solution;
(3)The preparation of need testing solution:Take health drink 10mL of the present invention, precision weighing, put in conical flask with cover, accurate Add methyl alcohol 10mL, close plug, weighed weight, ultrasonically treated 30min, let cool, more weighed weight, the weight of less loss is supplied with methyl alcohol Amount, shakes up, 0.45 μm of filtering with microporous membrane, takes subsequent filtrate, obtain final product need testing solution;
(4)Measure:Precision measures above-mentioned need testing solution, each 10 μ L of reference substance solution respectively, injects high performance liquid chromatography Instrument, is detected;
(5)Result:In every 10mL health drink of the present invention, malvidin content is 56.53 μ g.
Moreover, it will be appreciated that although this specification is been described by according to embodiment, not each embodiment only wraps Containing an independent technical scheme, only for clarity, those skilled in the art should for this narrating mode of specification Using specification as an entirety, the technical scheme in each embodiment can also form those skilled in the art through appropriately combined Understandable other embodiment.

Claims (4)

1. a kind of have the health drink promoting sleep function, improvement to have a sleepless night it is characterised in that this health drink is by following heavy The raw material of amount part is made:1 part of pilea mongolica, 1 part of Ailanthus altissima flower, this health drink is made up of following methods:Join by prescription weight Ratio takes pilea mongolica, Ailanthus altissima flower, plus 5~15 times of decoctings boil 1~2 hour, and the dregs of a decoction add 5 again~and that 10 times amount decoctings boil 0.5~1 is little When, decocting liquid merges, and filters, and filtrate concentrates, cooling, adds the ethanol that volumetric concentration is 95% to concentration of alcohol to be 60~75%, It is put in 4~8 DEG C after stirring and stands 12~48 hours, filter, filtrate recycling ethanol, obtain health care tea extract, with sucrose, add Water, sterilizing, make health drink.
2. health drink as claimed in claim 1 is it is characterised in that this health drink is made up of following methods:By prescription weight Proportioning takes pilea mongolica, Ailanthus altissima flower, plus 10 times of decoctings boil 1.5 hours, and the dregs of a decoction add 6 times amount decoctings again and boil 1 hour, decocting twice Liquid merges, and filters, and filtrate concentrates, cooling, adds the ethanol that volumetric concentration is 95% to be 70% to concentration of alcohol, is put in 5 after stirring DEG C standing 24 hours, filter, filtrate recycling ethanol, obtain health care tea extract, with sucrose, add water, sterilizing, make health beverage Material.
3. the quality determining method of health drink as claimed in claim 1 is it is characterised in that this health drink adopts following sides Method carries out quality testing:Using high effective liquid chromatography for measuring malvidin content:
(1)Chromatographic condition:Chromatographic column is C18 chromatographic column;With ratio for 40~60:40~60 methyl alcohol -0.15% phosphoric acid solution is Mobile phase;Detection wavelength 300~330nm, 25~45 DEG C of column temperature;
(2)The preparation of reference substance solution:Precision weighs malvidin reference substance and is placed in volumetric flask, plus methyl alcohol dissolves and is diluted to Scale, shakes up;Pipette above-mentioned solution and put volumetric flask, plus methanol constant volume, as reference substance stock solution;
(3)The preparation of need testing solution:Take health drink of the present invention, precision weighing, put in conical flask with cover, accurate addition first Alcohol, close plug, weighed weight, ultrasonically treated, let cool, more weighed weight, supply the weight of less loss with methyl alcohol, shake up, miillpore filter Filter, take subsequent filtrate, obtain final product need testing solution;
(4)Measure:Precision measures above-mentioned need testing solution, each 5~20 μ L of reference substance solution respectively, injects high performance liquid chromatography Instrument, is detected.
4. the quality determining method of health drink as claimed in claim 3 is it is characterised in that this health drink adopts following sides Method carries out quality testing:Using high effective liquid chromatography for measuring malvidin content:
(1)Chromatographic condition:Chromatographic column is C18 chromatographic column;With ratio for 58:42 methyl alcohol -0.15% phosphoric acid solution is mobile phase; Detection wavelength 328nm, 32 DEG C of column temperature;Number of theoretical plate is calculated by malvidin peak and should be not less than 3000;
(2)The preparation of reference substance solution:Precision weighs malvidin reference substance 10.00mg and is placed in 100mL volumetric flask, plus methyl alcohol Dissolve and be diluted to scale, shake up;Pipette above-mentioned solution 10mL and put 25mL volumetric flask, plus methanol constant volume, stock as reference substance Liquid;
(3)The preparation of need testing solution:Take health drink 10mL of the present invention, precision weighing, put in conical flask with cover, accurate addition Methyl alcohol 10mL, close plug, weighed weight, ultrasonically treated 30min, let cool, more weighed weight, supply the weight of less loss with methyl alcohol, shake Even, 0.45 μm of filtering with microporous membrane, take subsequent filtrate, obtain final product need testing solution;
(4)Measure:Precision measures above-mentioned need testing solution, each 10 μ L of reference substance solution respectively, injects high performance liquid chromatograph, enters Row detection.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107693636A (en) * 2017-10-31 2018-02-16 黑龙江民族职业学院 A kind of Chinese medicine composition for treating insomnia and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107693636A (en) * 2017-10-31 2018-02-16 黑龙江民族职业学院 A kind of Chinese medicine composition for treating insomnia and preparation method thereof
CN107693636B (en) * 2017-10-31 2021-06-22 黑龙江民族职业学院 Traditional Chinese medicine composition for treating insomnia and preparation method thereof

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