CN110179912A - A kind of preparation method and detection method of nourishing yin and lessening fire Chinese medicine composition - Google Patents

A kind of preparation method and detection method of nourishing yin and lessening fire Chinese medicine composition Download PDF

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CN110179912A
CN110179912A CN201910536691.XA CN201910536691A CN110179912A CN 110179912 A CN110179912 A CN 110179912A CN 201910536691 A CN201910536691 A CN 201910536691A CN 110179912 A CN110179912 A CN 110179912A
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chinese medicine
medicine composition
preparation
nourishing yin
rhizoma anemarrhenae
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陈炜
陈丽卿
韩俊琦
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HANGZHOU HUQINGYUTANG PHARMACEUTICAL INDUSTRY Co Ltd
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HANGZHOU HUQINGYUTANG PHARMACEUTICAL INDUSTRY Co Ltd
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Abstract

The invention discloses a kind of nourishing yin and lessening fire Chinese materia medica preparation and preparation method thereof and detection methods, comprising: (1) crushes tortoise plastron, Cortex Phellodendri and rhizoma anemarrhenae, obtain fine powder；(2) Cortex Phellodendri, rhizoma anemarrhenae and Rehmannia glutinosa are added water to cook, filtrate is obtained by filtration, concentrating filter liquor obtains thick paste；(3) pig spinal cord, which is set in boiling water, slightly boils, and removes crust, then mixes thoroughly with the fine powder and thick paste, various preparations are made.Compared with existing preparation method, the Chinese materia medica preparation dose is less, and has higher protective effect to hypoglycemia, meanwhile, there is better inhibiting effect to hyperglycemia.

Description

A kind of preparation method and detection method of nourishing yin and lessening fire Chinese medicine composition
Technical field
The invention belongs to field of Chinese medicinal composition, and in particular to a kind of preparation method and inspection of nourishing yin and lessening fire Chinese medicine composition Survey method.
Background technique
The Chinese medicine composition is the famous doctor's ZHU Dan-xi of Jin and Yuan dynasty according to " yin frequently in deficiency, yang frequently in excess, suitable Chang Yangqi Yin, yin is neat with sun, then water energy system is fiery, this is disease-free " the nourishing yin and lessening fire founded of theoretic knowledge represent prescription.To treat liver kidney The deficiency of Yin, osteopyrexia and fever caused by fire of deficiency type Kang Sheng is flushing to fire, and night sweat spermatorrhea, cough hemoptysis, dysphoria, that sufficient knee aches heat etc. is a variety of The important prescription of illness, it is significant in efficacy, paid attention to by doctor, and use till today.
Rehmannia glutinosa: nature and flavor are sweet, bitter, tepor, return liver and kidney channel, function nourishing yin and supplementing blood, beneficial to spirit and marrow.For the deficiency of liver-yin and kidney-yin, waist Knees soreness, osteopyrexia and fever, night sweat spermatorrhea, Heat Diabetes, blood deficiency chlorosis, palpitaition is seized with terror secondary, irregular menstruation, metrostaxis, dizziness, ear Ring, poliosis.Essentials of Matea Medica meaning " nourishing liver and kidney, nourishing the blood and yin, for agent on enriching blood." Compendium of Material Medica meaning: " replenishing essence marrow, Long muscle, promoting vital essence and blood genernation, tonifying five zang organs, internal injury is insufficient, promoting blood circulation, sharp knowledge, black beard and hair, man's general debility, threatened abortion in woman's wound, Wait for peacefully uncomfortable, tire produces all kinds of diseases and ailments ".
" drug justice " meaning: " radix rehmanniae preparata specially enters liver and enriches blood, radix rehmanniae preparata energy invigorating heart blood, more kidney tonifying water.Radix rehmanniae preparata five viscera settling and blood Arteries and veins moistens skin, nourishing the heart to keep a sound mind, and peaceful soul nourishes Kidney-Yin, packing marrow, is panacea." modern pharmacological research rehmanin containing Catalpol, Retinoid, carbohydrate and amino acid etc..Rehmannia glutinosa liquid extract has significant cardiac effect in experiment, and has diuresis.Also have Slight hypoglycemic effect.Glutinous rehmannia Liquor infusion significantly inhibits effect to rat formaldehyde arthritis.Also have anti-inflammatory granulation hyperplasia, The effect of exudation.
Tortoise plastron: nature and flavor, it is salty, sweet, slightly cold.Return liver, kidney, the heart channel of Hang-Shaoyin.Function nourishing and suppressing Yang, the strong bone of kidney-nourishing, blood-nourishing bushing.For Deficiency of Yin hectic fever, hectic fever due to yin night sweat, has a dizzy spell, endogenous deficient wind, and muscles and bones is withered soft, amnesia of having a guilty conscience.Zhu Zhenheng meaning: " tonifying yin, main negative blood are not Foot removes extravasated blood, and stop blooding dysentery, continuous muscles and bones control overstrain, limbs fatigue "." book on Chinese herbal medicine covers an aromatic plant metioned in ancient books " meaning: " special tonifying yin is empty, is apt to nourshing kidney damage "." guiding principle Mesh " meaning: " controlling waist foot to ache, bushing kidney, beneficial large intestine, only protracted dysentery is let out long, main difficult labour, subduing inflammation, ashing sickle sore "." medical center, which is usurped, to be wanted " Meaning: " bone hectic fever due to consumption is controlled, is spitted blood, bleeding from five sense organs or subcutaneous tissue, intestines wind hemorrhoid blood, the disease of YinXuXueRe." modern pharmacological research thinks that tortoise plastron has enriching yin pharmacology Effect, Sun Enting etc. studies the nourishing yin effect of tortoise plastron with microelement, and thinks that the upper and lower first of tortoise all has nourishing yin effect. Chen Meixiang etc. has investigated the toxicity of the upper and lower first of tortoise, it is believed that the toxicity of the upper and lower first of tortoise is extremely low, and " LD50 " is not measured.Xie Ping studies table The bright upper and lower first of tortoise contains 18 kinds of amino acid, inorganic salts, animal glue, cutin, protein, vitamin, chemistry of fats ingredient.
Cortex Phellodendri: nature and flavor, it is bitter, cold, return kidney, bladder meridian.Function heat-clearing and damp-drying drug, purging intense heat, except steaming, detoxification sore treatment.It is rushed down for damp and hot Dysentery, jaundice, leukorrhagia, heat gonorrhea, tinea pedis, osteopyrexia and fever, night sweat, spermatorrhea, sore swollen toxin, eczema itch.Stir-baked CORTEX PHELLODENDRI with salt solution nourishing yin and lessening fire is used In fire excess from yin deficiency, night sweat hectic fever due to yin.Shennong's Herbal carries Cortex Phellodendri and " ties heat, jaundice, perianal abscess, antidiarrheal dysentery, woman in main the five internal organs stomach Whitish metrorrhagia, acute vulva ulcer "." a supplement to augmented materia medica " meaning: " rhizoma anemarrhenae nourishing yin and lessening fire is obtained, rhizoma atractylodis is obtained except damp and clearing heat, is wanted to control to wither Medicine；It obtains asarum and rushes down bladder fire, control aphthae." " new compilation of materia medica " meaning: " Cortex Phellodendri, bitter cold micro-pungent, the yin that sinks decline, and rush down bladder phase Fire removes damp and clearing heat, burnt empty under treating, osteopyrexia and fever, all paralysis of withering, hot eyes tinnitus, jaundice of quenching one's thirst, and oedema is just closed, watery diarrhea hot dysentery, hemorrhoid Blood sausage wind, whitish metrorrhagia, all sore sufferings, head sore, aphtha, desinsection claming ascaris." modern pharmacology thinks that Cortex Phellodendri contains jamaicin, and has few The a variety of alkaloids of palmatine, phellodendrine, Palmatine of amount.In addition there are also nitrogen-free crystalline material (obakunone, obakulactones) And fat oil, mucilaginous substance sterols etc..Cortex Phellodendri has the effect of broad-spectrum antiseptic pharmacology；It can significantly and enduringly reduce blood pressure, to blood Platelet has protective effect；Play the role of promoting pancreatic secretion.
Rhizoma anemarrhenae: bitter in taste, sweet, cold, return lung, stomach, kidney channel.Function clearing heat-fire, fluid dryness are used for fever caused by exogenous pathogenic factors, high Hot polydipsia, lung-heat type cough, osteopyrexia and fever, Heat Diabetes, dry constipation of intestines.Shennong's Herbal meaning: " rhizoma anemarrhenae, bitter is cold, and main quench one's thirst is hankered, It removes pathogenic factor, limbs edema is lauched, tonifying for the deficiency, QI invigorating." " haigoushen " meaning: " vexed dry bored, the hot labor contact of bone, general debility during puerperium, kidney Gas labor, abhors dysphoria." Compendium of Material Medica meaning: " working hard for rhizoma anemarrhenae is cold and cool, under then moisten dry two enriching yin of kidney, on then clearing lung-heat gold and rush down Fire is two through gas drug dispensing.Cortex Phellodendri is then kidney channel blood system medicine, thus two medicines must mutual reinforcement between and go, all shrimps and jellyfish of people's ratio must be interdependent It is attached." " materia medica " meaning: " ancient book says that rhizoma anemarrhenae helps Cortex Phellodendri nourishing yin and lessening fire, there is the justice of mutual generation between metal and water ".The Baihu Tang of Zhong Jing, with knowing Mother is assistant gypsum, is the real heat for rushing down stomach meridian.Salt water profit training, downlink enters kidney, has that profit kidney is dry and the function of enriching yin.Contain steroid in rhizoma anemarrhenae Body saponin(e, flavones, lignanoid, polysaccharide, sterol and fat oil, mucilaginous substance etc..Modern pharmacological research proves that rhizoma anemarrhenae is made with antibacterial With heat-clearing effect, antiplatelet aggregative activity, hypoglycemic effect, sedation, rhizoma anemarrhenae, which matches Cortex Phellodendri, can reduce the emerging of nervous system Putting forth energy property.
Pig spinal cord: for the spinal cord of Suidae pig category animal pig.Nature and flavor are sweet, cold, flat.For osteopyrexia and fever, quench one's thirst, sore." guiding principle Mesh " meaning: " except children's infantile metopism, head sore and navel are swollen, eyebrow sore, the Psoralen marrow of clothes." " occupying diet spectrum with breath " meaning: " mends marrow yin-nourishing, controls bone Labor heat is steamed, with turbid spermatorrhea, the preferably food of aging." " book on Chinese herbal medicine is just read " meaning: " all deficiency of Yin hectic fever due to yin, five heart nights heat, rachiagia ridge is convex to wait diseases, It can all be used."
The Chinese medicine composition modern age is fire excess from yin deficiency for treating, and hyperactivity of yang due to yin deficiency is shown in the hemoptysis of pulmonary tuberculosis of disease, and climacteric is comprehensive Disease, the diseases such as old cognitive disorder.
It is significant in efficacy to feed back the Chinese medicine composition nourishing yin and lessening fire for market information in recent years, but this medicine taking dose larger (one Secondary 6g, 2-3 times on the one), it is not very convenient that patient and his family take, and limits the use of the medicine.Preferably to excavate and applying the Chinese medicine group Object is closed, we have invented a kind of preparation method, the Chinese medicine composition taking dose can be made to reduce 50%, not only convenient for taking, and And be also convenient for fully absorbing in vivo, to improve the curative effect of drug.We additionally provide the detection side of the Chinese medicine composition simultaneously Method, this method accuracy is high, favorable reproducibility, and stability is strong.
Summary of the invention
The present invention provides the preparation method and its detection method of a kind of nourishing yin and lessening fire Chinese medicine composition, which is obtained The Chinese medicine composition arrived has better protective action to hypoglycemia and hyperglycemia, and taking dose is smaller.
A kind of preparation method of nourishing yin and lessening fire Chinese medicine composition, comprising:
(1) tortoise plastron, Cortex Phellodendri and rhizoma anemarrhenae are crushed, obtains fine powder；
(2) Cortex Phellodendri, rhizoma anemarrhenae and Rehmannia glutinosa are added water to cook, filtrate is obtained by filtration, concentrating filter liquor obtains thick paste；
(3) pig spinal cord, which is set in boiling water, slightly boils, and removes crust, then mixes thoroughly with the fine powder and thick paste, dry, obtains described Chinese medicine composition.
In the present invention, the Chinese medicine composition can be prepared into various preparations, such as pill, capsule, granule, piece Agent etc..
Animal test results show when the mouse for hypoglycemia, using the use of the Chinese medicine composition of the method for the present invention When amount halves, there is essentially identical protective effect；Meanwhile when for hyperglycemia mouse, when dosage halves, there is preferably drop Blood glucose effect.
Preferably, the Chinese medicine composition is made of raw material from the following weight:
3-48 parts of rhizoma anemarrhenaes of Rehmannia glutinosa (salt stir-fry) 2-32 portions of Cortex Phellodendris 2-32 parts of (salt stir-fry) 3-48 parts of tortoise plastron (system) pig spinal cord 3-64 Part.
Preferably, in described pharmaceutical composition, Rehmannia glutinosa, rhizoma anemarrhenae, Cortex Phellodendri (salt stir-fry), tortoise plastron (system), pig spinal cord matter Amount is than being 6:4:4:6:8.
Preferably, the ratio between the dosage of Cortex Phellodendri and the dosage of Cortex Phellodendri in step (2) are 4:6 in step (1)；In step (1) The ratio between dosage of rhizoma anemarrhenae is 4:6 in rhizoma anemarrhenae and step (2).
Preferably, decocting 8~12 times that water used is medicinal material weight in step (2), decocting number is twice, often Secondary 1 hour.
In the present invention, the density of thick paste is 1.28~1.32 (90 DEG C), preferably, the density of thick paste is 1.30 (90 ℃)。
The present invention provides a kind of Chinese medicine compositions being prepared by the method.The composition enables effective component It is dissolved out to greatest extent, both absorbs human body adequately, also taking dose is made to reduce 50%, consequently facilitating patient It takes, while its pharmacological action for adjusting blood glucose is more significant.It can be used for nourishing yin and lessening fire, treat fire excess from yin deficiency card, such as yin The fire of deficiency type is prosperous, hyperactivity of yang due to yin deficiency is shown in the hemoptysis of pulmonary tuberculosis of disease, sex premature, climacteric syndrome, diabetes, the diseases such as old cognitive disorder Disease.
The present invention also provides the detection methods of the Chinese medicine composition described in one kind, comprising:
(1) Chinese medicine composition is finely ground, with methanol dissolution, test solution is obtained by filtration；
(2) high performance liquid chromatography sample introduction is used, the content of the small folds in a garment alkali of hydrochloric acid is measured, according to containing for the measured small folds in a garment alkali of hydrochloric acid Amount judges whether the Chinese medicine composition is qualified；
Mobile phase used in liquid chromatogram is the mixing of acetonitrile and phosphoric acid solution or the mixing of acetonitrile and ammonium acetate solution, The volume ratio of middle acetonitrile and phosphoric acid solution is 20~32:68~80；The volume ratio of acetonitrile and ammonium acetate solution be 20~30:70~ 80。
Preferably, the concentration of the phosphoric acid solution is 0.01~0.03mol/L；The concentration of the ammonium acetate solution is 0.03~0.05mol/L.
Compared with the existing technology, the beneficial effects of the present invention are embodied in:
(1) present invention is improved by the preparation method to the Chinese medicine composition, in the condition for reducing drug administration amount Under, improve protective effect of the drug to hypoglycemia and the preventive and therapeutic effect to hyperglycemia；
(2) detection method of the invention can carry out efficiently and accurately to the content of the active constituent of the pharmaceutical composition Detection, so that the quality to product is better controlled.
Detailed description of the invention
Fig. 1 is the liquid chromatogram of reference substance in embodiment 4；
Fig. 2 is the liquid chromatogram of test sample in embodiment 4.
Specific embodiment
Embodiment 1
Rehmannia glutinosa 480g rhizoma anemarrhenae (salt stir-fry) 320g Cortex Phellodendri (salt stir-fry) 320g tortoise plastron (system) 480g pig spinal cord 640g
The above five tastes, take tortoise plastron and Cortex Phellodendri 128g, and rhizoma anemarrhenae 128g is ground into fine powder, remaining Cortex Phellodendri, rhizoma anemarrhenae and Rehmannia glutinosa 12 times of amount water are added to decoct secondary, 1 hour every time, collecting decoction, filtration.It is about 1.30 (90 DEG C) that filtrate, which is concentrated into relative density, Thick paste, pig spinal cord, which is set in boiling water, slightly to be boiled, and is removed crust, is mixed thoroughly with above-mentioned fine powder and thick paste, be dried, crushed into fine powder, add 73.6g Refined honey and suitable water pill, film coating to get.
Embodiment 2
Rehmannia glutinosa 480g rhizoma anemarrhenae (salt stir-fry) 320g Cortex Phellodendri (salt stir-fry) 320g tortoise plastron (system) 480g pig spinal cord 640g
The above five tastes, take tortoise plastron and Cortex Phellodendri 160g, and rhizoma anemarrhenae 160g is ground into fine powder, remaining Cortex Phellodendri, rhizoma anemarrhenae and Rehmannia glutinosa 8 times of amount water are added to decoct secondary, 1 hour every time, collecting decoction, filtration.It is about 1.30 (90 DEG C) that filtrate, which is concentrated into relative density, Thick paste, pig spinal cord, which is set in boiling water, slightly to be boiled, and is removed crust, is mixed thoroughly with above-mentioned fine powder and thick paste, be dried, crushed into fine powder, add 73.6g Refined honey and suitable water pill, film coating to get.
Comparative example 1
Rehmannia glutinosa 120g rhizoma anemarrhenae (salt stir-fry) 80g Cortex Phellodendri (salt stir-fry) 80g tortoise plastron (system) 120g pig spinal cord 160g
The above five tastes, Rehmannia glutinosa, stir-baked CORTEX PHELLODENDRI with salt solution, tortoise plastron, rhizoma anemarrhenae are ground into coarse powder, and pig spinal cord, which is set in boiling water, slightly to be boiled, and remove outer Skin is mixed thoroughly with above-mentioned coarse powder, is dried, crushed into fine powder, is sieved, and is mixed, and adds refined honey and suitable water that pill is made.
It is about 480g that comparative example theory, which answers yield, and every gram is about 1.16g containing crude drug amount, and embodiment theory answers the yield to be about 1000g, every gram is about 2.24g containing crude drug amount.Embodiment taking dose reduces half (being kept to each 3g by each 6g), and takes Crude drug amount is basically unchanged.
Below by taking bolus of drug prepared by embodiment 1 and comparative example 1 as an example, it is described in detail.Application examples 1 is to the deficiency of Yin The protective effect that caused blood glucose reduces
Yin deficiency models preparation: experiment ICR system mouse, male, weight 18-24g.Thyroid tablet is ground into a powder and is added Enter to reserpine injection, the suspension of 7.5mg/ml containing thyroid tablet and reserpine 7.5mg/ml is made into 1%CMC-Na, often Its stomach-filling 0.4ml/20g weight, continuous 5 days.The activity of model group mouse is obvious less, in the back of a bow, roll up, dispirited, drinking-water and into Food substantially reduces, and excrement is half congealed and sticks in perianal, and weight is obviously lighter than Normal group.
7 groups of experiment mice point: 1) control group and 2) yin-deficient model control group, hello isometric water, 3) positive controls, six Taste Dihuang Wan 8g/kg；4) with 5) group be comparative example 1 it is small, large dosage of group, 4g/kg, 8g/kg；It 6) is that embodiment 1 is small, big with 7) group Dosage group 4g/kg, 8g/kg.Daily stomach-filling 1 time, continuous 5 days, gave moulding medicine to investigational agent, afternoon in the morning, except organizing 1) outer each group Moulding medicine is given, fasting 6h before last dose, 1h measuring blood sugar of blood extracting content after the last administration.
Influence (x ± s) of the table 1 to deficiency of Yin mouse blood sugar
N=10, compared with yin-deficient model control group: p < 0.01 * p < 0.05, * *
Seen from table 1, compared with Normal group, the blood-sugar content of yin-deficient model group is significantly reduced, pharmaceutical composition group In, pharmaceutical composition prepared by embodiment 1 has a significant protective effect to the reduction of blood glucose caused by the deficiency of Yin, and effect is substantially better than pair The pharmaceutical composition of 1 group of preparation of ratio.
Influence of the application examples 2 to diabetes hyperglycemia caused by alloxan
7 groups of experiment mice point: 1) control group and 2) alloxan model control group, hello isometric water, 3) positive control Group, Liuwei Dihuang Wan 8g/kg；4) with 5) group be comparative example 1 it is small, large dosage of group, 4g/kg, 8g/kg；It 6) is embodiment 1 with 7 groups Small, large dosage of group of 4g/kg, 8g/kg.Except 1) outer each group takes blood to survey to group with ip alloxan 200mg/kg, 72h after fasting 16h Blood glucose, the mouse by blood glucose in 10mmol/L or more are grouped at random, and daily stomach-filling 1 is administered once, and continuous 5 days, prohibit before last dose 15h is eaten, after the last administration 1h measuring blood sugar of blood extracting content.
Influence (x ± s) of the table 2 to alloxan mouse blood sugar
As can be seen from Table 2, the blood-sugar content of alloxan model group significantly increases, pharmaceutical composition compared with Normal group In object group, the pharmaceutical composition of example 1 group preparation has significant therapeutic effect to blood glucose rise caused by alloxan, and effect It is substantially better than the pharmaceutical composition of the preparation of comparative example 1.
The detection method of pharmaceutical composition prepared by the present invention is described below
The identification of pharmaceutical composition prepared by embodiment 3:
(1), this product is taken, microscopically observation, cellulose foresythia are set, peripheral cell prismatic crystal containing calcium oxalate is formed brilliant fine Dimension, the wall wood of crystal cell thicken.Irregular block piece lark, there are fine unity and coherence in writing or hole in surface.Needle-like calcium oxalate crystal bunchy Or it is dispersed in, long 26-110um.
(2), this product 1g is taken, it is finely ground, add methanol 20ml, be ultrasonically treated 30 minutes, filtration, filtrate is as test solution. Cortex Phellodendri control medicinal material 0.5g separately is taken, is made in the same way of control medicinal material solution.Berberine hydrochloride reference substance is taken again, and methanol is added to be made often Solution of the 1ml containing 0.5ml, as reference substance solution.It is tested according to thin-layered chromatography, draws test solution and control medicinal material is each 5ul, reference substance 1ul put respectively on same silica gel g thin-layer plate, with n-butanol-glacial acetic acid-water (7:1:2) for solvent, open up It opens, taking-up is dried, and is set and is inspected under ultraviolet lamp (365nm).In sample chromatogram, corresponding to reference substance and reference medicine chromatography Position on, show identical yellow fluorescence spot.
The assay (high performance liquid chromatography) of pharmaceutical composition effective component prepared by embodiment 4
Chromatographic condition and system suitability test:
Filler: octadecylsilane chemically bonded silica
Mobile phase: acetonitrile: 0.05mol/L ammonium acetate solution (30:70) (adjusting PH with glacial acetic acid is 4.0) is mobile phase
Detection wavelength: 349nm
Number of theoretical plate: 3000 should be not less than by calculating by Berberine hydrochloride peak
The preparation of reference substance solution: precision weighs that Berberine hydrochloride reference substance is appropriate, adds methanol that every 1ml is made containing 12 μ g's Solution, as reference substance solution.
The preparation of test solution: taking this product appropriate, finely ground, takes about 0.4g, accurately weighed, sets in 25ml volumetric flask, adds Methanol 20ml, ultrasonic treatment (power 120w, frequency 50kHz) 1 hour, lets cool, and adds methanol dilution to scale, shake up to get.
It is accurate respectively to measure reference substance solution and 20 μ l of test solution, inject liquid chromatograph, measurement.
With this condition, preferably, without peak is significantly interfered with, high sensitivity is reappeared for separation.Taste sampling test is lacked through Cortex Phellodendri to exist It is noiseless at λ=349nm.
The liquid chromatogram of reference substance solution is shown in that Fig. 1, the liquid chromatogram of test solution are shown in Fig. 2.
Embodiment 5
Chromatographic condition and system suitability test:
Filler: octadecylsilane chemically bonded silica
Mobile phase: acetonitrile: 0.02mol/L phosphoric acid solution (32:68)
Column temperature: room temperature
Flow velocity: 1.0ml/min
Detection wavelength: 245nm
Theoretical cam curve is calculated by Berberine hydrochloride peak should be not less than 4000
The preparation of reference substance solution: precision weighs that Berberine hydrochloride reference substance is appropriate, adds methanol that every 1ml is made containing 12 μ g's Solution, as reference substance solution.
The preparation of test solution: taking this product appropriate, finely ground, takes about 0.4g, accurately weighed, sets in 25ml volumetric flask, adds Methanol 20ml, ultrasonic treatment (power 120w, frequency 50kHz) 1 hour, lets cool, adds methanol dilution to scale, shake up, with 0.22 μ M miillpore filter filtration to get.
It is accurate respectively to measure reference substance solution and 20 μ l of test solution, inject liquid chromatograph, measurement.With this condition Berberine hydrochloride and other correlation peak-to-means can reach baseline separation, and characteristic peak retention time is 16 points or so at 20 DEG C of room temperature.
Embodiment 6
Precision Experiment
Above-mentioned contrast solution to be drawn, is repeated sample introduction 5 times, the relative standard deviation of Berberine hydrochloride peak area is 1.25%, As a result it is listed in table 3.
3 Precision test result of table
Experiment number Peak area RSD%
1 8364273
2 8456354
3 8237568 1.25
4 8513214
5 8427928
7 reappearance test of embodiment
6 parts of same sample lots are taken, are measured by sample test condition, the relative standard deviation of content of berberine hydrochloride is 2.43%, as a result it is listed in table 4.
4 reproducible test results of table
Table 4 the result shows that method of the invention reproducibility with higher.
8 recovery test of embodiment
Using sample-adding absorption method, the Chinese medicine composition of known content is taken, Berberine hydrochloride reference substance is added respectively, by above-mentioned Condition measurement, is as a result listed in table 5.
5 recovery test result of table
Table 5 the result shows that detection method of the invention has the preferable rate of recovery.

Claims (8)

1. a kind of preparation method of nourishing yin and lessening fire Chinese medicine composition characterized by comprising
(1) tortoise plastron, Cortex Phellodendri and rhizoma anemarrhenae are crushed, obtains fine powder；
(2) Cortex Phellodendri, rhizoma anemarrhenae and Rehmannia glutinosa are added water to cook, filtrate is obtained by filtration, concentrating filter liquor obtains thick paste；
(3) pig spinal cord, which is set in boiling water, slightly boils, and removes crust, then mixes thoroughly with the fine powder and thick paste, dry, obtains in described Drug composition.
2. the preparation method of nourishing yin and lessening fire Chinese medicine composition according to claim 1, which is characterized in that the Chinese medicine group Object is closed to be made of raw material from the following weight:
3-48 parts of rhizoma anemarrhenaes of Rehmannia glutinosa (salt stir-fry) 2-32 portions of Cortex Phellodendris 2-32 parts of (salt stir-fry) 3-48 parts of tortoise plastron (system) pig spinal cord 3-64 parts.
3. the preparation method of nourishing yin and lessening fire Chinese medicine composition according to claim 1, which is characterized in that yellow in step (1) The ratio between dosage of Cortex Phellodendri is 2:8~5:5 in the dosage of cypress and step (2)；
The ratio between rhizoma anemarrhenae and the dosage of rhizoma anemarrhenae in step (2) are 2:8~5:5 in step (1).
4. the preparation method of nourishing yin and lessening fire Chinese medicine composition according to claim 1, which is characterized in that in step (2), decoct 8~12 times that water used is medicinal material weight are boiled, decocting number is 1 hour every time twice.
5. the preparation method of nourishing yin and lessening fire Chinese medicine composition according to claim 1, which is characterized in that the density of thick paste is 1.28-1.32(90℃)。
6. a kind of Chinese medicine composition being prepared by the described in any item methods of Claims 1 to 5.
7. a kind of detection method of Chinese medicine composition as claimed in claim 6 characterized by comprising
(1) by the finely ground of the Chinese medicine composition, with methanol dissolution, test solution is obtained by filtration；
(2) high performance liquid chromatography sample introduction is used, the content of the small folds in a garment alkali of hydrochloric acid is measured, is sentenced according to the content of the measured small folds in a garment alkali of hydrochloric acid Whether the Chinese medicine composition that breaks is qualified；
Mobile phase used in liquid chromatogram is the mixing of acetonitrile and phosphoric acid solution or the mixing of acetonitrile and ammonium acetate solution, wherein second The volume ratio of nitrile and phosphoric acid solution is 20-32:68-80；The volume ratio of acetonitrile and ammonium acetate solution is 20-30:70-80.
8. the detection method of Chinese medicine composition according to claim 7, which is characterized in that the phosphoric acid solution solution or The concentration of ammonium acetate solution is 0.01~0.05mol/L.
CN201910536691.XA 2019-06-20 2019-06-20 A kind of preparation method and detection method of nourishing yin and lessening fire Chinese medicine composition Pending CN110179912A (en)

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Application publication date: 20190830