CN103169782B - A kind of tune stomach CHENGQI TANG granule and preparation method thereof and detection method - Google Patents
A kind of tune stomach CHENGQI TANG granule and preparation method thereof and detection method Download PDFInfo
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- CN103169782B CN103169782B CN201310123884.5A CN201310123884A CN103169782B CN 103169782 B CN103169782 B CN 103169782B CN 201310123884 A CN201310123884 A CN 201310123884A CN 103169782 B CN103169782 B CN 103169782B
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Abstract
The invention provides a kind of tune stomach CHENGQI TANG granule and preparation method thereof and detection method, the described rheum officinale of tune stomach CHENGQI TANG granule by 2 parts by weight and the Radix Glycyrrhizae boiling of 1 parts by weight, the saltcake adding 1.5 parts by weight after merging filtrate dissolves, and granulates and obtain after dry; Described detection method comprises the following steps: identify described tune stomach CHENGQI TANG granule by thin-layered chromatography; The content of beary metal in described tune stomach CHENGQI TANG granule is measured by Residue on ignition check method; The Residual Levels of Organochlorine Pesticides in described tune stomach CHENGQI TANG granule is measured by persticide residue determination method; By adjusting the finger-print of stomach CHENGQI TANG granule described in high effective liquid chromatography for measuring; The extract content of described tune stomach CHENGQI TANG granule is measured by hot dipping; By adjusting the content of material in stomach CHENGQI TANG granule described in high effective liquid chromatography for measuring.Preparation method of the present invention is simple, and detection method can control the quality of this granule effectively.
Description
Technical field
The invention belongs to the field of Chinese medicines.Be specifically related to Chinese medicinal granule and preparation method thereof and detection method, particularly relate to a kind of tune stomach CHENGQI TANG granule and preparation method thereof and detection method.
Background technology
Adjust stomach CHENGQI TANG to go out self-evident Fang Xian work Wonderful Well-Tried Recipes, be made up of rheum officinale (five money) Radix Glycyrrhizae (three money) saltcake (money half), upper work one takes, water two clock, decocts to a clock, clothes before food.There is the function of slow lower thermojunction, cure mainly Yangming disease gastrointestine dryness heat card.Suffer from constipation, thirsty vexed, hectic fever, or turgor in abdomen, or be delirious speech, tongue fur true yellow, slippery and rapid pulse; And stomach and intestine heat contain and cause send out a spot tell nosebleed, ability to speak abscess of throat etc.Side's Chinese medicine only three tastes, right compatibility is appropriate: rheum officinale bitter cold, with expelling pathogenic heat to loosen the bowels, cleanses stomach; Saltcake is salty-cold to rush down lower heat extraction, softening mass and moistening dryness; Capture with honey-fried licorice root mediation rheum officinale, saltcake the side that expels the heat-evil, make it gentle.Zou Shu cloud we itself so name adjusts stomach CHENGQI TANG, its merit of holding gas is all rheum officinale.Compared with our and large and small CHENGQI TANG, lead stagnant side under rushing down weak, be especially suitable for disease gently weakling.Due to originally can harmonizing intestine-stomach, hold along stomach Qi, drive away stomach accumulated heat, make stomach Qi must be with, mechanism of qi connects, thus all cards are removed, therefore named tune stomach CHENGQI TANG.
Adjust stomach CHENGQI TANG to be one of classic prescriptions for the treatment of YangmingFushi syndrome in Zhang Zhongjing treatise on Febrile Diseases, original text the 248th article is said: " Taiyin diseases three days, sweating is not understood, swallow heat of evaporation person, belongs to stomach yet, tune stomach CHENGQI TANG master it." describe the interpretation of the cause, onset and process of an illness and the symptom feature of the party's idicatio, can be regarded as the generality of exchanging stomach CHENGQI TANG main symptom and describe.This external " sun section " the 29th article and Yangming disease the 207th article mention two kinds of instructions about how to take medicine of the party respectively, are not quite similar although symptom describes, and its basic pathogenesis is all that because of stomach-heat and dryness very therefore constipation is all consistent.Instructions about how to take medicine there is the difference of " taking it less less " and " clothes ", but be all " to warmly take ".The main syndrome of the party has summed up following several: 1. typhoid fever sun clear proof, not aversion to cold, and fear of heat on the contrary, thirstyly just closes, and delirious speech abdomen is full, the dry reality of middle Jiao; 2. typhoid fever tells rear distention and fullness in the abdomen; 3. Yangming disease can not be told any more and vexed: disappear 4. kind food and urinating.Analyze Fang Yi, wherein rheum officinale bitter cold according to its composition, heat extraction swings reality; Saltcake is salty-cold, moistening for dryness and softening hard mass; Radix Glycyrrhizae is sweet slow, makes it unlikely and injures one's stomach, therefore is called tune stomach CHENGQI TANG.Can find out, why the effect of this prescription is different from large Xiao Chengqi Tang, just be that " dry " that its effect main points concentrate in the middle of the clinical YangmingFushi syndrome for the treatment of " ruffian, full, dry, real " is demonstrate,proved, Main Function is soft heavily fortified point, saltcake is namely utilized in enteron aisle, to form the effect of hyperosmosis as mineral salt composition, moisture in the middle of intestines wall surrounding tissue is drawn in the middle of enteron aisle as far as possible, to help too dry stool to be softened, thus is excreted.The effect of Radix Glycyrrhizae is to protect stomach in temperature, coordinating the drug actions of a prescription, therefore generally should use honey-fried licorice root.Rheum officinale act as logical under, principal feature is to strengthen enterocinesia, promotes stool and discharges downwards, if but do not have the saltcake of q.s to attract moisture around intestines wall to enteron aisle, stool is not softened fully, still efficient solution can not remove the problem of constipation.Therefore our compatibility is appropriate, taste application can also be added if desired.
Pharmacological action shows to adjust stomach CHENGQI TANG to mainly contain antibacterial action.In vitro Bactericidal Experiments confirms, adjusts stomach CHENGQI TANG stoste and concentrate all to have certain antibacterial action to staphylococcus.Rheum officinale, saltcake have discharge function, and Radix Glycyrrhizae has detoxication.Owing to adjusting the kind slow lower thermojunction of stomach CHENGQI TANG merit, cure mainly the illness that stomach accumulated heat causes.The many bed brakings of orthopedics and traumatology patient, normal taste are dull, and clinical manifestation is that gastral cavity abdomen ruffian is full, do not feel like eating, and belch is done frequently, very then keeps vomiting, if stagnant heat-transmission also has gastral cavilty dysphoria, diseases such as disliking pantothenic acid of vomitting, clinical available tune stomach CHENGQI TANG clearing away heat to ease the stomach, conditioning Central Region.Though adjust in stomach CHENGQI TANG side and also have rheum officinale, saltcake, decoct together with Radix Glycyrrhizae and rheum officinale, under its merit is slow, alleviate the property under the rushing down of rheum officinale.Modern pharmacology research shows, after rheum officinale and Radix Glycyrrhizae are decocted together, tannin (astringent component) decocting rate of mensuration increases.If see that clinical wound is eaten less afterwards, indigestion and loss of appetite person, available tune stomach CHENGQI TANG is with " regulating stomach-QI ".Its ancient modern Application comprehensive and result of study known, the party is with a wide range of applications.
Chinese medicinal granule is under guidance of traditional Chinese medicine theory, with the prepared slices of Chinese crude drugs of specification Preparation process for raw material, adopt extract, the technology such as low temperature concentrates, wink-dry and the granule made.It both can supply clinical flexible prescription, and allotment is taken after mixing it with water, and can be used as again the raw material of industry of Chinese medicine preparation, also for tcm clinical practice medication provides new approach.Compared with traditional Chinese herbs decoction, the advantage of Compatible Granule keeps the nature and flavor feature of original Chinese medicine, remain the characteristic of differentiation of tcm, rational production technology is developed according to the character of Chinese medicine, formulate advanced feasible quality control standard, be processed into as regulation and standardization, industrialized modern Chinese herbal medicine preparation.Overcome traditional Chinese medicine decoction decoct time-consuming, to take inconvenience, technique extensive and lack the drawbacks such as quality control, adapted to the demand of modern social development.
The Chinese medicinal granule of current application is greatly mainly with the unit prepared slices of Chinese crude drugs particle that unit Chinese medicine is made by modern pharmaceutical technique, and existing hundreds of units medicine materical crude slice granule goes on the market.Although but Chinese medicinal granule has lot of advantages, in making and clinical practice, also there is many drawbacks, with traditional in the principal mode traditional Chinese herbal decoction of medical drugs still there is certain gap.Traditional Chinese herbal decoction is that compound compatibility is decocted and formed, the not simple addition of the chemical composition of single medicinal material in the side of being equal to of the material base of its clinical efficacy, but the interactional synthesis result of various chemical composition.Single medicinal material granule mixed dissolution does not have whole effective constituents of " group's medicine is decocted altogether "; the granule prepared by existing technique in other words can not comprise the effective constituent of middle medical drugs requirement completely; cause traditional prescription working substance basis to change, so that existing granule medication can not be equal to traditional traditional Chinese herbal decoction.Finally may cause the change of clinical efficacy or the change of pharmacological action.
The advantage of Chinese medicinal granule, at compound, is hereby controlled according to TCM differentiation opinion, with the needs demonstrate,proving prescription, by the new formulation particle that traditional classical prescription medicine employing modern science and technology is refined.Its nature and flavor, return through and effect and former prescription be substantially consistent, not adding or few sugaring, antiseptic and other excipient, is a kind ofly take into account the new model decocting traditional classical prescription of two features with card tunes side and compound conjunction.Chinese medicine compound prescription is the marrow of clinical performance curative effect, really embody " diagnosis and treatment based on an overall analysis of the illness and the patient's condition, with side make up a prescription, compound close decoct " tcm clinical practice administration features.But, the application method of traditional Chinese medicine " medicine materical crude slice is used as medicine, and faces with decocting soup " and the series of problems brought thus, what day by day show with Modern Live is incompatible, and the present situation of prepared slices of Chinese crude drugs quality allows of no optimist, become the obstacle of traditional Chinese medicine sustainable development.Under the background of the market demand huge at home and abroad and Japan, the fast-developing single in Taiwan and herbal mixture concentrated granular, Chinese medicine compound prescription granule has been developed and has been classified as National Key Research Programs Xiang by the Ministry of Science and Technology and State Administration of Traditional Chinese Medicine, its objective is reply Post-WTO China medicinal industry and the severe challenge of facing, accelerate the scientific and technical innovation of medicinal industry, realize the modernization of Chinese medicine.Therefore, to the research of Chinese medicine composite powdered extracts, there is larger value.
Summary of the invention
Therefore, the object of the invention is for the tune stomach CHENGQI TANG granule existed in prior art and Modern Live incompatible, and each flavour of a drug are simply added the deficiency brought when single granule is taken, and the deficiency that quality can not control well, there is provided a kind of and adjust stomach CHENGQI TANG granule and preparation method thereof and detection method, this tune stomach CHENGQI TANG granule gives full play to the requirement of drug matching, be suitable for Modern Live, preparation method is simple, and by this detection method can be safer use.
Unless specifically stated otherwise, " test sample " herein all refers to adjust stomach CHENGQI TANG granule.
Unless specifically stated otherwise, " benzene hexachloride " herein all refers to hexachlorocyclohexanes.
Unless specifically stated otherwise, " D.D.T. (dichloro-diphenyl-trichloroethane) " herein all refers to biconjugate chlorphenyl trichloroethanes.
Unless specifically stated otherwise, " ppm " herein all refer to 1,000,000/.
For above-mentioned purpose, technical scheme provided by the invention is as follows:
On the one hand, the invention provides a kind of tune stomach CHENGQI TANG granule, the described rheum officinale of tune stomach CHENGQI TANG granule by 2 parts by weight and the Radix Glycyrrhizae boiling of 1 parts by weight, the saltcake adding 1.5 parts by weight after merging filtrate dissolves, granulate after dry and obtain, preferably, described Radix Glycyrrhizae is honey-fried licorice root.
On the other hand, the invention provides the preparation method of the tune stomach CHENGQI TANG granule described in a kind of the invention described above, said method comprising the steps of:
Take the rheum officinale of 2 parts by weight and the Radix Glycyrrhizae of 1 parts by weight, boiling is extracted 1 ~ 3 time, extracts 1 ~ 2 hour at every turn; The saltcake adding 1.5 parts by weight after merging filtrate dissolves, then is condensed into medicinal extract, after drying, granulates, to obtain final product.
Preferably, extract 2 times.
Preferably, each extraction 1 hour, also preferably, every gram of rheum officinale and Radix Glycyrrhizae add 6 ~ 10ml water extraction and get.
Preferably, first time extracts every gram of rheum officinale and Radix Glycyrrhizae and adds 10ml water extraction and get, or second time is extracted every gram of rheum officinale and Radix Glycyrrhizae and added 8ml water extraction and get.
Preferably, described drying is microwave drying.
Also on the one hand, the invention provides the detection method of the tune stomach CHENGQI TANG granule described in a kind of the invention described above, described detection method comprises the following steps:
Step 1: identify described tune stomach CHENGQI TANG granule by thin-layered chromatography;
Step 2: measure the content of beary metal in described tune stomach CHENGQI TANG granule by Residue on ignition check method;
Step 3: measure the Residual Levels of Organochlorine Pesticides in described tune stomach CHENGQI TANG granule by persticide residue determination method;
Step 4: by adjusting the finger-print of stomach CHENGQI TANG granule described in high effective liquid chromatography for measuring;
Step 5: the extract content being measured described tune stomach CHENGQI TANG granule by hot dipping;
Step 6: by adjusting the content of material in stomach CHENGQI TANG granule described in high effective liquid chromatography for measuring.
Preferably, described step 1 comprises the following steps:
1) rheum officinale sample solution group and Radix Glycyrrhizae sample solution group is prepared, described rheum officinale sample solution group comprises rheum officinale need testing solution, rheum officinale control medicinal material solution and Chrysophanol reference substance solution, more preferably, described rheum officinale sample solution group also comprises rheum officinale negative sample solution, and described rheum officinale negative sample is the sample lacking rheum officinale by adjusting the technology preparation of stomach CHENGQI TANG granule to prepare; Described Radix Glycyrrhizae sample solution group comprises Radix Glycyrrhizae need testing solution, Radix Glycyrrhizae control medicinal material solution and Radix Glycyrrhizae crude drug solution, described Radix Glycyrrhizae crude drug is separately with the sample that Radix Glycyrrhizae is prepared by the technology preparation of tune stomach CHENGQI TANG granule, more preferably, described Radix Glycyrrhizae sample solution group also comprises Radix Glycyrrhizae negative sample solution, and described Radix Glycyrrhizae negative sample is the sample lacking Radix Glycyrrhizae by adjusting the technology preparation of stomach CHENGQI TANG granule to prepare;
2) rheum officinale sample solution group put respectively and put on same silica gel g thin-layer plate respectively on same silica gel g thin-layer plate, by Radix Glycyrrhizae sample solution group, add developping agent and launch, taking-up is dried, and sprays with developer to spot development, detects, to obtain final product.
Preferably, described rheum officinale need testing solution is obtained by the method comprised the following steps:
Get described tune stomach CHENGQI TANG granule, porphyrize, solubilizer dissolves, and puts in water-bath and adds hot reflux, after cooling, filters, filtrate evaporate to dryness, and residue adds ethanol and dissolves, and to obtain final product; More preferably, get described tune stomach CHENGQI TANG granule 2 ~ 8g, preferably get 5g, further preferably, described solvent is methylene chloride 10 ~ 50ml and hydrochloric acid 0.1 ~ 2ml, is preferably methylene chloride 30ml and hydrochloric acid 1ml, again preferably, add hot reflux 10 ~ 50 minutes, preferably add hot reflux 30 minutes; Also preferably, residue adds 0.5 ~ 2.0ml ethanol and dissolves, and preferably adds 1ml ethanol and dissolves; Further preferably, described rheum officinale negative sample solution is obtained by the method identical with rheum officinale need testing solution, preferably gets described rheum officinale negative sample 1 ~ 5g;
Or preferably, described rheum officinale control medicinal material solution is obtained by the method comprised the following steps:
Get rheum officinale control medicinal material, add methylene chloride and hydrochloric acid, then make rheum officinale control medicinal material solution according to the method identical with described rheum officinale need testing solution; More preferably, rheum officinale control medicinal material 0.5 ~ 2.0g is got; Preferably get 1g, further preferably, add methylene chloride 5 ~ 20ml, hydrochloric acid 0.5 ~ 2.0ml; Also preferably, add methylene chloride 10ml, hydrochloric acid 1ml;
Or preferably, described Chrysophanol reference substance solution, by getting Chrysophanol reference substance, adds ethanol and makes every 1ml and obtain containing the solution of 0.1 ~ 1.0mg Chrysophanol reference substance, preferably make the solution of every 1ml containing 0.5mg Chrysophanol reference substance;
Or preferably, described Radix Glycyrrhizae need testing solution is obtained by the method comprised the following steps:
Get described tune stomach CHENGQI TANG granule, be dissolved in water, the jolting that then adds diethyl ether is extracted, then discards ether solution, and water layer extracts with normal butyl alcohol jolting again, merges normal butyl alcohol liquid, evaporate to dryness, and residue adds methyl alcohol and dissolves, and to obtain final product; More preferably, get described tune stomach CHENGQI TANG granule 2 ~ 8g, preferably get described tune stomach CHENGQI TANG granule 5g; Further preferably, add the water-soluble solution of 10 ~ 30ml, preferably add the water-soluble solution of 20ml; Again preferably, add diethyl ether extraction 1 ~ 3 time, adds 10 ~ 30ml ether at every turn, preferably extracts 2 times, add 20ml ether at every turn; Also preferably, add normal butyl alcohol and extract 2 times, add 5 ~ 20ml normal butyl alcohol at every turn, preferably add 15ml; Further preferably, residue adds 0.5 ~ 1.5ml methyl alcohol and dissolves, and preferably adds 1ml methyl alcohol; Further preferably, described Radix Glycyrrhizae negative sample solution is obtained by the method identical with Radix Glycyrrhizae need testing solution, preferably gets described Radix Glycyrrhizae negative sample 1 ~ 5g;
Or preferably, described Radix Glycyrrhizae control medicinal material solution is obtained by the method comprised the following steps:
Extracting Radix Glycyrrhizae control medicinal material, adds alcohol heating reflux, filters, filtrate evaporate to dryness, and residue adds methyl alcohol and dissolves, and to obtain final product; More preferably, extracting Radix Glycyrrhizae control medicinal material 0.5 ~ 3.0g, preferred extracting Radix Glycyrrhizae control medicinal material 1g, further preferably, adds ethanol 10 ~ 30ml, preferably adds ethanol 20ml; Also preferably, heating and refluxing extraction 0.5 ~ 3 hour, preferably extracts 1 hour; Again preferably, residue adds 0.5 ~ 1.5ml methyl alcohol, preferably adds 1ml;
Or preferably, described Radix Glycyrrhizae crude drug solution is obtained by the method identical with Radix Glycyrrhizae need testing solution, preferably gets described Radix Glycyrrhizae crude drug 1 ~ 5g:
Preferably, described rheum officinale sample solution group is with sherwood oil-ethyl formate-formic acid for developping agent launches, and more preferably, the volume ratio of described sherwood oil-ethyl formate-formic acid PetroChina Company Limited. ether, ethyl formate and formic acid is 15:5:1; Inspect under preferably putting 365nm uviol lamp;
Or preferably, described Radix Glycyrrhizae sample solution group with acetic ether-methanoic acid-glacial acetic acid-water for developping agent, more preferably, in described acetic ether-methanoic acid-glacial acetic acid-water, the volume ratio of ethyl acetate, formic acid, glacial acetic acid and water is 15: 1: 1: 2, and described developer is preferably the ethanol solution of sulfuric acid of 10 volume %.
Preferably, in step 2, the content of beary metal≤25ppm recorded.
Preferably, in step 3, described organo-chlorine pesticide is benzene hexachloride, D.D.T. (dichloro-diphenyl-trichloroethane) and pentachloronitrobenzene (PCNB), the content≤0.20ppm of described benzene hexachloride; Content≤the 0.20ppm of described D.D.T. (dichloro-diphenyl-trichloroethane), the content≤0.10ppm of described pentachloronitrobenzene.
Preferably, described step 4 or 6 is undertaken by the method comprised the following steps:
Prepare testing sample solution, pass through high effective liquid chromatography for measuring.
Preferably, take octadecylsilane chemically bonded silica as filling agent; More preferably, when finger-print by adjusting stomach CHENGQI TANG granule described in high effective liquid chromatography for measuring, take methyl alcohol as mobile phase A, 0.3 volume % phosphoric acid is Mobile phase B, carries out gradient elution by following condition:
0 to 20 minute: the concentration of mobile phase A at the uniform velocity becomes 35 volume % from 20 volume %, and Mobile phase B concentration at the uniform velocity becomes 65 volume % from 80 volume %;
20 to 50 minutes: the concentration of mobile phase A at the uniform velocity becomes 50 volume % from 35 volume %, and Mobile phase B concentration at the uniform velocity becomes 50 volume % from 65 volume %;
50 to 85 minutes: the concentration of mobile phase A at the uniform velocity becomes 80 volume % from 50 volume %, and Mobile phase B concentration at the uniform velocity becomes 20 volume % from 50 volume %;
85 to 102 minutes: the concentration of mobile phase A is 80 volume %, and Mobile phase B concentration is 20 volume %; Or
More preferably, when content by adjusting material in stomach CHENGQI TANG granule described in high effective liquid chromatography for measuring, take methyl alcohol as mobile phase A, 0.1 volume % phosphoric acid is Mobile phase B, and the volume ratio of mobile phase A and Mobile phase B is 80:20;
More preferably, determined wavelength is 254nm, and also preferably, number of theoretical plate calculates should be not less than 3000 by archen peak;
Also preferably, when measuring the content of material in described tune stomach CHENGQI TANG granule, described testing sample solution is obtained by the method comprised the following steps:
Get described tune stomach CHENGQI TANG granule and reference substance makes need testing solution and reference substance solution respectively; Preferably, described reference substance comprises archen reference substance and/or Chrysophanol reference substance;
Also preferably, when measuring finger-print, described testing sample solution comprises need testing solution and reference substance solution; Preferably, described reference substance comprises archen reference substance, Chrysophanol reference substance, Rhein reference substance and/or ammonium glycyrrhetate reference substance; Preferably, described testing sample solution also comprises control medicinal material solution, and described control medicinal material comprises rheum officinale control medicinal material, Radix Glycyrrhizae control medicinal material and saltcake control medicinal material;
Further preferably, described need testing solution is obtained by the method comprised the following steps:
Get described tune stomach CHENGQI TANG granule, put in tool plug conical flask, add methanol solution, close plug, weighed weight, ultrasonic process, cooling, more weighed weight, supply the weight of less loss, shake up with methyl alcohol, filters, get subsequent filtrate, to obtain final product; Preferably get described tune stomach CHENGQI TANG granule 0.5 ~ 3.0g, also preferably get described tune stomach CHENGQI TANG granule 1.0g, more preferably, add methanol solution 10 ~ 30ml, preferably add methanol solution 25ml, also preferably, ultrasonic process 15 ~ 35 minutes, preferred ultrasonic process 20 minutes;
Or further preferably, described reference substance solution is obtained by the method comprised the following steps:
Get reference substance appropriate, add methanol solution and make the solution of 1ml containing 5 ~ 20 μ g reference substances, preferably make the solution of 1ml containing 10 μ g reference substances;
Or further preferably, described control medicinal material solution is obtained by the method comprised the following steps:
Get control medicinal material appropriate, add methyl alcohol, weighed weight, ultrasonic process, place room temperature, supply the weight of less loss with methyl alcohol, filter, get subsequent filtrate, to obtain final product; Again preferably, add methyl alcohol 10 ~ 30ml, preferably add methyl alcohol 25ml, also preferably, ultrasonic process 15 ~ 35 minutes, preferred ultrasonic process 20 minutes;
Preferably, mass percentage content >=33.9% of extract in described step 5.
Preferably, similarity >=0.90 of test sample finger-print and reference substance finger-print.
Record according to former side, adjust stomach CHENGQI TANG to cure mainly Yangming disease gastrointestine dryness heat card.For suffering from constipation, thirsty vexed, hectic fever, or turgor in abdomen, or be delirious speech, tongue fur true yellow, slippery and rapid pulse; And stomach and intestine heat contain and cause send out a spot tell nosebleed, ability to speak abscess of throat.Therefore its function is cured mainly be described as: Yangming disease gastrointestine dryness heat is demonstrate,proved.For suffering from constipation, thirsty vexed, hectic fever, or turgor in abdomen, or be delirious speech, tongue fur true yellow, slippery and rapid pulse; And stomach and intestine heat contain and cause send out a spot tell nosebleed, ability to speak abscess of throat.
This granule, for formula, should be followed the doctor's advice, and specifically describes to be: for formula, follow the doctor's advice.
According to production technology, clinical application situation, determine that the packing specification adjusting stomach CHENGQI TANG granule is every packed 5g, every 1 gram is equivalent to 2.6g medicine materical crude slice.
Former side decocts twice by the every agent of traditional method of administration, takes at twice, and particle 10g is made in the every agent of we, press an often packed dose, therefore packing specification is decided to be every packed 5g.
According to holding conditions under " Chinese Pharmacopoeia " version in 2010 granule and medicinal material medicinal extract kind item, sealing, dry place preserves.
The term of validity of this granule is 24 months, prescription: rheum officinale 1200g Radix Glycyrrhizae 600g saltcake 900g, makes 1000g particle.
Stomach CHENGQI TANG is adjusted to cure mainly Yangming disease gastrointestine dryness heat card.Suffer from constipation, thirsty vexed, hectic fever, or turgor in abdomen, or be delirious speech, tongue fur true yellow, slippery and rapid pulse; And stomach and intestine heat contain and cause send out a spot tell nosebleed, ability to speak abscess of throat etc.Modern pharmacology shows to adjust stomach CHENGQI TANG all to have certain antibacterial action to staphylococcus.And after rheum officinale and Radix Glycyrrhizae are decocted together, tannin (astringent component) decocting rate of mensuration increases.If see that clinical wound is eaten less afterwards, indigestion and loss of appetite person, available tune stomach CHENGQI TANG is with " regulating stomach-QI ".Its ancient modern Application comprehensive and result of study known, the party is with a wide range of applications.
Tune stomach CHENGQI TANG granule of the present invention makes granule after traditionally closing and decocting, and gives full play to the advantage of drug matching, embodies traditional Chinese medicine organic conception, overcomes each flavour of a drug when current single granule is taken and is simply added the deficiency brought; Establish the quality standard adjusting stomach CHENGQI TANG granule perfect, effectively can control the quality of this granule; Adjust stomach CHENGQI TANG granule to be convenient to patient to portably use and store, on using, eliminate the trouble of decoction; Greater significance is had to promotion TCM Modernization.
Preparation method of the present invention: its method is simple, with low cost, is applicable to suitability for industrialized production.It is by crude drug medicine materical crude slice extracting in water, and microwave drying, collects dry cream, granulates, the Chinese medicinal granule of packing, and this particle can directly provide compatibility in prescriptions of traditional Chinese medicine to use.The tune stomach CHENGQI TANG granule that this method is produced maintains the whole features adjusting stomach CHENGQI TANG, its effective constituent, nature and flavor, Gui Jing, cure mainly, effect adjusts the agent of stomach CHENGQI TANG consistent with tradition, and the effective constituent of single quality is controlled preferably; It can ensure monarch that the traditional Chinese medical science is traditional, minister, helps, make and the feature of diagnosis and treatment based on an overall analysis of the illness and the patient's condition, flexibly plus-minus, eliminate again the trouble of patient's traditional decoction simultaneously, have do not need to decoct, directly take after mixing it with water, dose is few, effect is rapid, composition is complete, determined curative effect, safety and sanitation and carry many advantages such as preservation facilitates.
Detection method of the present invention: shown by concrete testing data, the present invention is a kind of feasible Components identification and content assaying method, the discrimination method specificity adopted is strong, assay accuracy is high, favorable reproducibility, for production unit and testing agency provide Testing index, detection means and technical method etc., with can better Instructing manufacture, make controlling of production process more rationally strict, in process of producing product, the quality of product effectively can be controlled with this measuring method, thus guarantee clinical efficacy and the security of adjusting stomach CHENGQI TANG granule thing.
Accompanying drawing explanation
Below, describe embodiment of the present invention in detail by reference to the accompanying drawings, wherein:
Fig. 1 is the preparation technology figure of tune stomach CHENGQI TANG granule of the present invention;
Fig. 2 is the thin-layer chromatography chromatogram of rheum officinale sample solution group of the present invention, wherein, Fig. 2 a is the thin-layer chromatography chromatogram of the described rheum officinale sample solution group of inspecting under daylight lamp, Fig. 2 b is the thin-layer chromatography chromatogram of the described rheum officinale sample solution group of inspecting under 365nm ultraviolet light, Fig. 2 c is after ammonia steam is smoked, the thin-layer chromatography chromatogram of the described rheum officinale sample solution group of inspecting under light, Fig. 2 d is after ammonia steam is smoked, the thin-layer chromatography chromatogram of the described rheum officinale sample solution group of inspecting under 365nm ultraviolet light, in figure, 1-3 is test sample, 4 is rheum officinale control medicinal material solution, 5 is Chrysophanol reference substance, 6 is rheum officinale negative sample,
Fig. 3 is the thin-layer chromatography chromatogram of Radix Glycyrrhizae sample solution group of the present invention, wherein, Fig. 3 a is the thin-layer chromatography chromatogram of the described Radix Glycyrrhizae sample solution group of inspecting under daylight lamp, Fig. 3 b is the thin-layer chromatography chromatogram of the described Radix Glycyrrhizae sample solution group of inspecting under 365nm ultraviolet light, in figure, 1 is Radix Glycyrrhizae control medicinal material, and 2 is Radix Glycyrrhizae crude drug, and 3-5 is test sample, 6 is Radix Glycyrrhizae negative sample;
Fig. 4 is the finger-print of tune stomach CHENGQI TANG granule of the present invention;
Fig. 5 is the high-efficient liquid phase chromatogram of blank solvent ethanol of the present invention;
Fig. 6 is the finger-print of Rhein reference substance of the present invention;
Fig. 7 is the finger-print of archen reference substance of the present invention;
Fig. 8 is the finger-print of Chrysophanol reference substance of the present invention;
Fig. 9 is the finger-print of ammonium glycyrrhetate reference substance of the present invention;
Figure 10 is the finger-print of rheum officinale control medicinal material of the present invention;
Figure 11 is the finger-print of Radix Glycyrrhizae control medicinal material of the present invention;
Figure 12 is the finger-print of saltcake control medicinal material of the present invention;
Figure 13 is the specificity test findings in the embodiment of the present invention 7, and wherein, Figure 13 a is the high-efficient liquid phase chromatogram of archen reference substance; Figure 13 b is the high-efficient liquid phase chromatogram of Chrysophanol reference substance; Figure 13 c is the high-efficient liquid phase chromatogram of tune stomach CHENGQI TANG granule of the present invention; Figure 13 d is the high-efficient liquid phase chromatogram of rheum officinale negative sample;
Figure 14 is the canonical plotting of archen of the present invention and Chrysophanol, and wherein, Figure 14 a is the canonical plotting of archen, and Figure 14 b is the canonical plotting of Chrysophanol.
Embodiment
Unless specifically stated otherwise, rheum officinale lot number used in following examples is 110713201, Sichuan, the place of production; Radix Glycyrrhizae is honey-fried licorice root, and lot number is 110606121, the Inner Mongol, the place of production; Saltcake lot number is 110712141, Qinghai, the place of production.
Unless specifically stated otherwise, reagent used in following examples is analytical reagent, and can be commercially available from regular channel.
embodiment 1 adjusts the preparation of stomach CHENGQI TANG granule
1. crude drug source
Source and the place of production are in table 1.
Table 1
2. instrument and equipment
HWZ-5B-1 box-type microwave vacuum drying device, sky wawter bloom circle pharmaceutical equipment Science and Technology Ltd.; RE-5205 type Rotary Evaporators, Shanghai Yarong Biochemical Instrument Plant.
3. preparation method
Get rheum officinale, Radix Glycyrrhizae boiling twice, filter, merging filtrate, filtrate adds saltcake and dissolves after boiling, 70 DEG C of reduced pressure concentrations, be concentrated into the clear cream that relative density is 1.05 ~ 1.10 (60 DEG C), microwave drying, microwave power is 5Kw, temperature of charge 50 DEG C, working time is 20min, and drying obtains dry cream particle, and process chart is shown in Fig. 1.
Actual conditions is as shown in table 2 below:
Table 2
Take rhubarb medicinal material 120g in prescription ratio, licorice medicinal materials 60g, saltcake 90g, numbering 1 ~ 9, by L
9(3
4) orthogonal arrage arrangement test, test findings is in table 3:
Table 3 L
9(3
4) orthogonal experiments
The content analysis of variance table of table 4 archen
| Soruces of variation | Sum of square of deviations | Degree of freedom | F value | F critical value | Conspicuousness |
| A | 0.06 | 2 | 3.09 | 19 | |
| B | 0.01 | 2 | 0.37 | 19 | |
| C | 0.01 | 2 | 0.29 | 19 | |
| Error | 0.00 | 2 |
The content analysis of variance table of table 5 Chrysophanol
| Soruces of variation | Sum of square of deviations | Degree of freedom | F value | F critical value | Conspicuousness |
| A | 0.07 | 2 | 3.40 | 19 | |
| B | 0.00 | 2 | 0.06 | 19 | |
| C | 0.00 | 2 | 0.03 | 19 | |
| Error | 0.00 | 2 | 0.5 |
The analysis of variance table of table 6 dry spun
| Soruces of variation | Sum of square of deviations | Degree of freedom | F value | F critical value | Conspicuousness |
| A | 26.48 | 2 | 1324.08 | 19 | |
| B | 3.13 | 2 | 156.30 | 19 | |
| C | 0.07 | 2 | 3.27 | 19 | |
| Error | 0.55 | 2 |
Thus, show from the above results, process conditions are: A
2b
2c
2time archen, the content of Chrysophanol and dry cream of spraying yield higher; Comprehensive above-mentioned analysis of experiments, reduces the angle of energy consumption from industrialized production, under ensureing the prerequisite of effective component content, amount of water first time is 10 volume times amount, second time 8 volume times amount.
4. obtained dry leaching powder result
Table 7 extract result table
| Extract | Proterties | Extracted amount (g) | Extraction ratio (%) |
| Dry extract | Tawny; The micro-perfume (or spice) of gas, bitter | 155.2 | 36.5 |
Dry extract was pulverized 80 mesh sieves, stomach CHENGQI TANG granule powder 155.2g must be adjusted.
embodiment 2 thin-layered chromatography identifies that embodiment 1 is A in process conditions
2
b
2
c
2
time obtained tune
stomach CHENGQI TANG granule
1. adjust the discriminating of rheum officinale in stomach CHENGQI TANG granule
1.1 medicinal materials and reagent
Rheum officinale control medicinal material: lot number is 120984-200301, is purchased from Nat'l Pharmaceutical & Biological Products Control Institute.
Chrysophanol reference substance: lot number is 110796-201017, is purchased from Nat'l Pharmaceutical & Biological Products Control Institute.
Test sample: 12011001 is A according to embodiment 1 in process conditions by Kangmei Pharmaceutical Co., Ltd
2b
2c
2time method obtain.
Thin layer plate: silica G plate, is made by oneself by Kangmei Pharmaceutical Co., Ltd.
1.2 test procedure
The preparation of rheum officinale need testing solution: get and adjust stomach CHENGQI TANG granule 2.5g, porphyrize, the 30ml that adds methylene chloride, hydrochloric acid 1ml, put in water-bath and add hot reflux 30 minutes, let cool, and filter, filtrate evaporate to dryness, residue adds ethanol 1ml makes dissolving, as need testing solution;
The preparation of rheum officinale control medicinal material solution: get rheum officinale control medicinal material 1.0050g, the 5ml that adds methylene chloride, hydrochloric acid 0.5ml, make control medicinal material solution with need testing solution method for making;
The preparation of Chrysophanol reference substance solution: get Chrysophanol reference substance 1.230mg, adds methyl alcohol and makes the reference substance solution of 1ml containing Chrysophanol 0.1023mg.
The preparation of rheum officinale negative sample solution: get 1g and lack rheum officinale by the sample adjusting the technology preparation of stomach CHENGQI TANG granule to prepare; Rheum officinale negative sample solution is made according to the method identical with rheum officinale need testing solution.
Thin layer plate: silica G plate;
Point sample amount: each 8 μ l;
Point sample mode: spot application;
Developping agent: the upper solution of sherwood oil (30 ~ 60 DEG C)-ethyl formate-formic acid (15: 5: 1) is developping agent, exhibition, to about 13cm, is taken out, is dried;
Develop the color and inspect: inspecting under putting ultraviolet lamp (365nm), putting after smoking in ammonia steam, inspect under putting daylight.
Result: in test sample chromatogram, on the position corresponding to control medicinal material chromatogram, aobvious five identical fluorescent orange spots; On the position corresponding to reference substance chromatogram, the fluorescence spot of aobvious same color; Put after smoking in ammonia steam, inspect under putting daylight, spot becomes redness.See Fig. 2.
2. adjust the discriminating of Radix Glycyrrhizae in stomach CHENGQI TANG granule
2.1 medicinal materials and reagent
Radix Glycyrrhizae control medicinal material: lot number is 120934-200608, is purchased from Nat'l Pharmaceutical & Biological Products Control Institute.
Test sample: 12011002 is A according to embodiment 1 in process conditions by Kangmei Pharmaceutical Co., Ltd
2b
2c
2time method obtain.
Thin layer plate: 1% NaOH silica G plate, is made by oneself by Kangmei Pharmaceutical Co., Ltd.
2.2 test procedure
The preparation of Radix Glycyrrhizae need testing solution: get and adjust stomach CHENGQI TANG granule 5.0g, the 20ml that adds water makes dissolving, the jolting that adds diethyl ether extracts 2 times, and each 20ml, discards ether solution, water layer extracts 2 times with normal butyl alcohol jolting again, each 15ml, merges normal butyl alcohol liquid, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as Radix Glycyrrhizae need testing solution.
The preparation of Radix Glycyrrhizae control medicinal material solution: extracting Radix Glycyrrhizae control medicinal material 0.9930g, adds ethanol 20ml, adds hot reflux 1 hour, and filter, filtrate evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as Radix Glycyrrhizae control medicinal material solution.
The preparation of Radix Glycyrrhizae crude drug solution: get separately with the sample 1g that Radix Glycyrrhizae is prepared by the technology preparation of tune stomach CHENGQI TANG granule, make Radix Glycyrrhizae crude drug solution according to the method identical with Radix Glycyrrhizae need testing solution.
The preparation of Radix Glycyrrhizae negative sample solution: get and lack Radix Glycyrrhizae by the sample 1g adjusting the technology preparation of stomach CHENGQI TANG granule to prepare, make Radix Glycyrrhizae negative sample solution according to the method identical with Radix Glycyrrhizae need testing solution.
Thin layer plate: 1% NaOH silica G plate;
Point sample amount: each 5 μ l;
Point sample mode: spot application;
Developping agent: acetic ether-methanoic acid-glacial acetic acid-water (15: 1: 1:2) is developping agent, exhibition, to about 13cm, is taken out, is dried;
Developer: volume percent content is the ethanol solution of sulfuric acid of 10%, 105 DEG C are heated to clear spot;
Inspect: inspect under putting daylight, inspect under putting ultraviolet lamp (365nm).
Result: in test sample chromatogram, on the position corresponding to control medicinal material chromatogram, aobvious identical yellow colored speckles; Under 365nm ultraviolet light, on the position corresponding to reference substance chromatogram, the fluorescence spot of aobvious same color.See Fig. 3.
it is A that embodiment 3 detects embodiment 1 in process conditions
2
b
2
c
2
time obtained tune stomach CHENGQI TANG join
the content of beary metal of side's particle
Detection is with reference under Chinese Pharmacopoeia version in 2010 coptis bolus for clearing the upper heat [inspection] item, the tune stomach CHENGQI TANG granule got by the method for embodiment 1 is obtained is about 1g(lot number 12011003, made by oneself by Kangmei Pharmaceutical Co., Ltd), accurately weighed, blazing to complete ashing according to Residue on ignition check method (Chinese Pharmacopoeia version in 2010 annex Ⅸ J).Get the residue left over, check (Chinese Pharmacopoeia version in 2010 annex Ⅸ E second method), result shows, is no more than 25/1000000ths containing heavy metal in accordance with the law.
it is A that embodiment 4 detects embodiment 1 in process conditions
2
b
2
c
2
time obtained tune stomach CHENGQI TANG join
the Residual Levels of Organochlorine Pesticides of side's particle
Get by the obtained tune stomach CHENGQI TANG granule of the method for embodiment 1 that (lot number 20120109 is A according to embodiment 1 in process conditions by Kangmei Pharmaceutical Co., Ltd
2b
2c
2time obtained), measure according to persticide residue determination method (determination of residual amount of Chinese Pharmacopoeia version in a 2010 annex Ⅸ Q organic chlorine agriculture chemicals), result shows, benzene hexachloride (total BHC) is no more than 2/10000000ths; D.D.T. (dichloro-diphenyl-trichloroethane) (total DDT) is no more than 2/10000000ths; Pentachloronitrobenzene (PCNB) is no more than 1/10000000th.
Other every regulations relevant under meeting Chinese Pharmacopoeia version in 2010 annex I C granule item.
it is A that embodiment 5 measures embodiment 1 in process conditions
2
b
2
c
2
time obtained tune stomach CHENGQI TANG join
the finger-print of side's particle
1. instrument and reagent
1.1 instrument high performance liquid chromatographs: Waters2695-2489, Empower2Personal Single System SW chem workstation; Chromatographic column: Waters symmetry
c18 (4.6mm × 250mm, 5 μm); Electronic analytical balance: METTER TOLEDO XP6; HANGPING FA2104; Supersonic extractors: KQ-300VDB type double frequency numerical control ultrasonic cleaning instrument.
1.2 reagent methyl alcohol are chromatographically pure, and water is ultrapure water; It is pure that other reagent are analysis.
(lot number: 12010903 is A according to embodiment 1 in process conditions to the tune stomach CHENGQI TANG granule prepared by the method described in embodiment 1 of 1.3 reagents
2b
2c
2time obtained); The contrast of single medicinal material comprises rheum officinale, Radix Glycyrrhizae, saltcake; Archen (Nat'l Pharmaceutical & Biological Products Control Institute, lot number: 110756-200110); Chrysophanol (Nat'l Pharmaceutical & Biological Products Control Institute, lot number: 110796-201017); Rhein (Nat'l Pharmaceutical & Biological Products Control Institute, lot number: 0756-200206); Ammonium glycyrrhetate (Nat'l Pharmaceutical & Biological Products Control Institute, lot number: 110731-200511).
2. chromatographic condition and system suitability test take octadecylsilane chemically bonded silica as filling agent; Take methyl alcohol as mobile phase A, 0.3 volume % phosphoric acid is Mobile phase B, and the regulation according to the form below 8 carries out wash-out; Determined wavelength is 254nm.Number of theoretical plate calculates should be not less than 3000 by archen peak.
Stomach CHENGQI TANG finger-print HPLC eluent gradient adjusted by table 8
The preparation of 3 solution
The preparation of 3.1 reference substance solution gets archen, Chrysophanol, Rhein and ammonium glycyrrhetate reference substance in right amount, accurately weighed, adds methanol solution and makes the solution of every 1ml containing 10ug, filter, to obtain final product.
The preparation of 3.2 need testing solutions is got and is adjusted stomach CHENGQI TANG granule powder 1.0g, accurately weighed, puts in tool plug conical flask, adds methanol solution 25ml, close plug, weighed weight, ultrasonic process 20 minutes, lets cool, more weighed weight, supplies the weight of less loss with methyl alcohol, shake up, filter, get subsequent filtrate, to obtain final product.
The preparation of 3.3 rhubarb medicinal material contrast solutions prepares rhubarb medicinal material reference substance by tune stomach CHENGQI TANG granule method for making, get 0.6g, accurately weighed, put in conical flask, precision adds methyl alcohol 25ml, weighed weight, ultrasonic process 20 minutes, places room temperature, the weight of less loss is supplied with methyl alcohol, filter, get subsequent filtrate, to obtain final product.
The preparation of 3.4 licorice medicinal materials contrast solutions prepares licorice medicinal materials reference substance by tune stomach CHENGQI TANG granule method for making, get 0.4g, accurately weighed, put in conical flask, precision adds methyl alcohol 25ml, weighed weight, ultrasonic process 20 minutes, places room temperature, the weight of less loss is supplied with methyl alcohol, filter, get subsequent filtrate, to obtain final product.
The preparation of 3.5 saltcake medicinal material contrast solutions prepares saltcake Authentic plant drugs by tune stomach CHENGQI TANG granule method for making, get 0.4g, accurately weighed, put in conical flask, precision adds methyl alcohol 25ml, weighed weight, ultrasonic process 20 minutes, places room temperature, the weight of less loss is supplied with methyl alcohol, filter, get subsequent filtrate, to obtain final product.
Determination method is accurate respectively draws reference substance solution and each 10 μ l of need testing solution, injection liquid chromatography, measures, to obtain final product.
Result, as shown in Fig. 4-12, illustrates similarity >=0.90 of test sample finger-print and reference substance finger-print, and in known sample, the belongingness of main active is better, and specificity is better.
it is A that embodiment 6 measures embodiment 1 in process conditions
2
b
2
c
2
time obtained tune stomach CHENGQI TANG join
the extract of side's particle
Get by the obtained tune stomach CHENGQI TANG granule powder 2g of the method for embodiment 1, accurately weighed, precision adds ethanol 100ml, measure according to the hot dipping (Chinese Pharmacopoeia version in 2010 annex Ⅹ A) under ethanol soluble extractives determination method item, result shows, the mass percentage content of its extract is no less than 33.9%.
Table 9 ethanol soluble extractives measurement result
The mean value of the measurement result of three batch samples is 42.49%, and by 80% conversion of mean value, the mass percentage content of extract is no less than 33.9%.
it is A that embodiment 7 measures embodiment 1 in process conditions
2
b
2
c
2
time obtained tune stomach CHENGQI TANG join
content of material-methodological study in side's particle
1, instrument and reagent
1.1 instruments: high performance liquid chromatograph: Waters2695-2489, Empower2Personal Single System SW chem workstation; Chromatographic column: Agilent XDB-C18 (4.6mm × 250mm, 5 μm); Electronic analytical balance: XP6, FA2104; Supersonic extractors: KQ300VDB.
1.2 reagent: methyl alcohol is chromatographically pure, water is ultrapure water; It is pure that other reagent are analysis.
1.3 reagents: (lot number: 12010903 is A according to embodiment 1 in process conditions to adjust stomach CHENGQI TANG granule
2b
2c
2time obtained): archen (solid preparation of traditional Chinese medicine manufacturing technology national project center, lot number: 1038-040521); Chrysophanol (Nat'l Pharmaceutical & Biological Products Control Institute, lot number: 110796-201017).
2, chromatographic condition and system flexibility take octadecylsilane chemically bonded silica as filling agent; With methyl alcohol-0.1 volume % phosphoric acid solution (80: 20) for mobile phase; Determined wavelength is 254nm; Column temperature 35 DEG C; Number of theoretical plate calculates should be not less than 3000 by archen peak.
3, the preparation of solution
The preparation precision of 3.1 reference substance solution takes archen, Chrysophanol reference substance is appropriate, accurately weighed, adds methyl alcohol and dissolves, and makes every 1ml containing archen reference substance 0.02mg, containing the solution of Chrysophanol reference substance 0.01mg, filters, to obtain final product.
The preparation of 3.2 need testing solutions is got and is adjusted stomach CHENGQI TANG granule appropriate, porphyrize, mixing, about get 1g, accurately weighed, put in tool plug conical flask, precision adds methyl alcohol 25ml, weighed weight, ultrasonic process (power 270W, frequency 45KHz) 20min, let cool, weighed weight again, supplies the weight of less loss, shakes up with methyl alcohol, filter, get subsequent filtrate, as need testing solution.
4, Method validation
4.1 accuracy test
(lot number: 12010903 is A according to embodiment 1 in process conditions to get the same batch sample of known content
2b
2c
2in time, obtains, content: 0.03%) 6 parts, get about 0.5g for every part, accurately weighed, precision adds archen, Chrysophanol reference substance mixed solution (concentration is respectively 0.1513mg/ml, 0.0773mg/ml) 2ml respectively, by method under [assay] item, prepare need testing solution, sample introduction measures, and calculates the recovery, the results are shown in Table 10-1 and table 10-2.
Table 10-1 archen accuracy determination test findings (n=6)
Table 10-2 Chrysophanol accuracy determination test findings (n=6)
This law recovery is good as seen from the above table, is suitable as the assay of this product.
4.2 precision test
4.2.1 replica test: get with a collection of tune stomach CHENGQI TANG granule that (lot number: 12010903 is A according to embodiment 1 in process conditions
2b
2c
2time obtained), by legal system below [assay] item for basic, normal, high 3 concentration (being equivalent to 50% of test concentrations, 100%, 150%), each concentration 3 increment product, totally 9 increment product, measure archen, Chrysophanol peak content respectively, the results are shown in Table 11.
Table 11 replica test result (n=9)
This law repeatability is good as seen from the above table, meets the requirement of assay.
4.2.2 precision test: get and adjust stomach CHENGQI TANG granule (lot number: 12010903 is A according to embodiment 1 in process conditions
2b
2c
2time obtained) need testing solution, by above-mentioned chromatographic condition, repeat sample introduction 6 times, measure archen, Chrysophanol peak area, the results are shown in Table 12.
Table 12 Precision test result
This law precision is good as seen from the above table, meets the requirement of assay.
4.3 specificity tests
Lack the negative sample of rhubarb medicinal material by recipe quantity preparation, make negative solution by the preparation method of need testing solution.Obtain the chromatographic fractionation figure of reference substance, sample, negative sample by above chromatographic condition, in negative sample chromatogram, with archen, Chrysophanol retention time relevant position is noiseless, and peak occurs.The results are shown in Figure 13.
4.4 linear relationship
The above-mentioned archen of accurate absorption, Chrysophanol contrast liquid each 2, 5, 10, 15, 20 μ l, peak area is measured by above-mentioned chromatographic condition, with respective peak area score value respectively to archen, Chrysophanol concentration carries out recurrence process, draw archen, the regression equation of Chrysophanol is respectively y=3520.48x-27198.66, r=1, y=3049.45x-23367.61, r=1 the results are shown in Figure 14, the concentration showing the peak area of archen in the scope of 2 ~ 20 μ g/ml and reference substance is good linear relationship, the concentration of the peak area of Chrysophanol in the scope of 2 ~ 20 μ g/ml and reference substance is good linear relationship.
4.5 study on the stability
(lot number: 12010903 is A according to embodiment 1 in process conditions to get same tune stomach CHENGQI TANG granule
2b
2c
2time obtained) test liquid, drew 20 μ l by above-mentioned chromatographic condition respectively at the 0th, 2,4,6,8,10 and 12 hour and measure.Result shows, test sample mensuration solution peak area value in 12h is basically identical, and the RSD of need testing solution is respectively 1.23%, 1.06% (n=6), and test sample measures in solution 12h stable.
Table 13-1 stability test result (archen)
Table 13-2 stability test result (Chrysophanol)
5, sample size measures
Get 6 batches and adjust stomach CHENGQI TANG granule, by drafting content assaying method operation, measuring the content of material archen wherein, Chrysophanol, the results are shown in Table 14.
Stomach CHENGQI TANG granule assay result adjusted by table 14
| Lot number | Emodin content (mg/g) | Determination of chrysophanol (mg/g) |
| 12010901 | 0.28 | 0.21 |
| 12010902 | 0.32 | 0.24 |
| 12010903 | 0.32 | 0.24 |
| 12011001 | 0.27 | 0.19 |
| 12011002 | 0.32 | 0.23 |
| 12011003 | 0.32 | 0.24 |
6, the determination of content limit
Content limit calculates by assay result 80%, and therefore every bag contains rheum officinale with archen (C
15h
10o
5) meter be no less than 1.2mg, with Chrysophanol (C
15h
10o
4) meter, be no less than 0.88mg.
Claims (21)
1. adjust the detection method of stomach CHENGQI TANG granule for one kind, the described rheum officinale of tune stomach CHENGQI TANG granule by 2 parts by weight and the Radix Glycyrrhizae boiling of 1 parts by weight, the saltcake adding 1.5 parts by weight after merging filtrate dissolves, and granulate after dry and obtain, described detection method comprises the following steps:
Step 1: identify described tune stomach CHENGQI TANG granule by thin-layered chromatography;
Step 2: measure the content of beary metal in described tune stomach CHENGQI TANG granule by Residue on ignition check method;
Step 3: measure the Residual Levels of Organochlorine Pesticides in described tune stomach CHENGQI TANG granule by persticide residue determination method;
Step 4: by adjusting the finger-print of stomach CHENGQI TANG granule described in high effective liquid chromatography for measuring;
Step 5: the extract content being measured described tune stomach CHENGQI TANG granule by hot dipping;
Step 6: by adjusting the content of material in stomach CHENGQI TANG granule described in high effective liquid chromatography for measuring;
Wherein, described step 4 is undertaken by the method comprised the following steps:
Prepare testing sample solution, pass through high effective liquid chromatography for measuring;
Take octadecylsilane chemically bonded silica as filling agent;
Take methyl alcohol as mobile phase A, 0.3 volume % phosphoric acid is Mobile phase B, carries out gradient elution by following condition:
0 to 20 minute: the concentration of mobile phase A at the uniform velocity becomes 35 volume % from 20 volume %, and Mobile phase B concentration at the uniform velocity becomes 65 volume % from 80 volume %;
20 to 50 minutes: the concentration of mobile phase A at the uniform velocity becomes 50 volume % from 35 volume %, and Mobile phase B concentration at the uniform velocity becomes 50 volume % from 65 volume %;
50 to 85 minutes: the concentration of mobile phase A at the uniform velocity becomes 80 volume % from 50 volume %, and Mobile phase B concentration at the uniform velocity becomes 20 volume % from 50 volume %;
85 to 102 minutes: the concentration of mobile phase A is 80 volume %, and Mobile phase B concentration is 20 volume %;
Determined wavelength is 254nm, and number of theoretical plate calculates should be not less than 3000 by archen peak;
Described testing sample solution comprises need testing solution and reference substance solution, and described reference substance comprises archen reference substance, Chrysophanol reference substance, Rhein reference substance and/or ammonium glycyrrhetate reference substance; Described testing sample solution also comprises control medicinal material solution, and described control medicinal material comprises rheum officinale control medicinal material, Radix Glycyrrhizae control medicinal material and saltcake control medicinal material;
Wherein, described need testing solution is obtained by the method comprised the following steps: get described tune stomach CHENGQI TANG granule 0.5 ~ 3.0g, accurately weighed, put in tool plug conical flask, add methanol solution 10 ~ 30ml, close plug, weighed weight, ultrasonic process 15 ~ 35 minutes, cooling, weighed weight again, supply the weight of less loss with methyl alcohol, shake up, filter, get subsequent filtrate, to obtain final product;
Described reference substance solution is obtained by the method comprised the following steps: get reference substance appropriate, adds methanol solution and makes the solution of 1ml containing 5 ~ 20 μ g reference substances;
Described control medicinal material solution is obtained by the method comprised the following steps: get control medicinal material appropriate, add methyl alcohol 10 ~ 30ml, weighed weight, ultrasonic process 15 ~ 35 minutes, places room temperature, supplies the weight of less loss with methyl alcohol, filters, gets subsequent filtrate, to obtain final product.
2. the detection method of tune stomach CHENGQI TANG granule according to claim 1, wherein, described step 1 comprises the following steps:
1) rheum officinale sample solution group and Radix Glycyrrhizae sample solution group is prepared, described rheum officinale sample solution group comprises rheum officinale need testing solution, rheum officinale control medicinal material solution and Chrysophanol reference substance solution, described Radix Glycyrrhizae sample solution group comprises Radix Glycyrrhizae need testing solution, Radix Glycyrrhizae control medicinal material solution and Radix Glycyrrhizae crude drug solution, and described Radix Glycyrrhizae crude drug is separately with the sample that Radix Glycyrrhizae is prepared by the technology preparation of tune stomach CHENGQI TANG granule;
Described rheum officinale need testing solution is obtained by the method comprised the following steps: get described tune stomach CHENGQI TANG granule 2 ~ 8g, porphyrize, 10 ~ the 50ml and hydrochloric acid 0.1 ~ 2ml that adds methylene chloride dissolves, put in water-bath and add hot reflux 10 ~ 50 minutes, after cooling, filter, filtrate evaporate to dryness, residue adds 0.5 ~ 2.0ml ethanol and dissolves, and to obtain final product;
Described rheum officinale control medicinal material solution is obtained by the method comprised the following steps: get rheum officinale control medicinal material 0.5 ~ 2.0g, add methylene chloride 5 ~ 20ml, hydrochloric acid 0.5 ~ 2.0ml, then make rheum officinale control medicinal material solution according to the method identical with described rheum officinale need testing solution;
Described Chrysophanol reference substance solution obtains by the following method: get Chrysophanol reference substance, adds ethanol and makes the solution of every 1ml containing 0.1 ~ 1.0mg Chrysophanol reference substance;
Described Radix Glycyrrhizae need testing solution is obtained by the method comprised the following steps: get described tune stomach CHENGQI TANG granule 2 ~ 8g, add the water-soluble solution of 10-30ml, then the jolting that adds diethyl ether is extracted 1 ~ 3 time, adds 10 ~ 30ml ether at every turn, then discards ether solution, water layer extracts 2 times with normal butyl alcohol jolting again, add 5 ~ 20ml normal butyl alcohol at every turn, merge normal butyl alcohol liquid, evaporate to dryness, residue adds 0.5 ~ 1.5ml methyl alcohol and dissolves, and to obtain final product;
Described Radix Glycyrrhizae control medicinal material solution is obtained by the method comprised the following steps: extracting Radix Glycyrrhizae control medicinal material 0.5 ~ 3.0g, adds ethanol 10 ~ 30ml heating and refluxing extraction 0.5 ~ 3 hour, filters, filtrate evaporate to dryness, and residue adds 0.5 ~ 1.5ml methyl alcohol and dissolves, and to obtain final product;
Described Radix Glycyrrhizae crude drug solution is obtained by the method identical with Radix Glycyrrhizae need testing solution;
2) rheum officinale sample solution group put on same silica gel g thin-layer plate respectively, adding volume ratio is that the sherwood oil-ethyl formate-formic acid of 15:5:1 launches as developping agent, and taking-up is dried, and inspects under putting 365nm uviol lamp;
Radix Glycyrrhizae sample solution group is put on same silica gel g thin-layer plate respectively, add volume ratio be 15: 1: 1: 2 acetic ether-methanoic acid-glacial acetic acid-water launch as developping agent, taking-up is dried, spray with developer to spot development, described developer is the ethanol solution of sulfuric acid of 10 volume %, detects, to obtain final product.
3. the detection method of tune stomach CHENGQI TANG granule according to claim 1, wherein, described Radix Glycyrrhizae is honey-fried licorice root.
4. the detection method of tune stomach CHENGQI TANG granule according to claim 2, wherein, in the preparation method of rheum officinale need testing solution described in described step 1, described tune stomach CHENGQI TANG granule is 5g; Methylene chloride is 30ml, and hydrochloric acid is 1ml; Add hot reflux 30 minutes; Residue adds 1ml ethanol and dissolves.
5. the detection method of tune stomach CHENGQI TANG granule according to claim 2, wherein, in the preparation method of the solution of rheum officinale control medicinal material described in described step 1, getting rheum officinale control medicinal material is 1g; Add methylene chloride 10ml, hydrochloric acid 1ml.
6. the detection method of tune stomach CHENGQI TANG granule according to claim 2, wherein, Chrysophanol reference substance solution described in described step 1, by getting Chrysophanol reference substance, adds ethanol and makes the solution of every 1ml containing 0.5mg Chrysophanol reference substance.
7. the detection method of tune stomach CHENGQI TANG granule according to claim 2, wherein, the group of rheum officinale sample solution described in described step 1 also comprises rheum officinale negative sample solution, and described rheum officinale negative sample is the sample lacking rheum officinale by adjusting the technology preparation of stomach CHENGQI TANG granule to prepare; Described rheum officinale negative sample solution is obtained by the method identical with rheum officinale need testing solution.
8. the detection method of tune stomach CHENGQI TANG granule according to claim 7, wherein, gets described rheum officinale negative sample 5g.
9. the detection method of tune stomach CHENGQI TANG granule according to claim 2, wherein, in the preparation method of Radix Glycyrrhizae need testing solution described in described step 1, gets described tune stomach CHENGQI TANG granule 5g; Add the water-soluble solution of 20ml; Add diethyl ether extraction 2 times, adds 20ml ether at every turn; Add normal butyl alcohol 15ml jolting to extract; Residue adds 1ml methyl alcohol and dissolves.
10. the detection method of tune stomach CHENGQI TANG granule according to claim 2, wherein, in the preparation method of the solution of Radix Glycyrrhizae control medicinal material described in described step 1, extracting Radix Glycyrrhizae control medicinal material 1g; Add ethanol 20ml heating and refluxing extraction 1 hour; Residue adds 1ml methyl alcohol.
The detection method of 11. tune stomach CHENGQI TANG granules according to claim 2, wherein, in the preparation method of the solution of Radix Glycyrrhizae crude drug described in described step 1, gets described Radix Glycyrrhizae crude drug 5g.
The detection method of 12. tune stomach CHENGQI TANG granules according to claim 2, wherein, the group of Radix Glycyrrhizae sample solution described in described step 1 also comprises Radix Glycyrrhizae negative sample solution, described Radix Glycyrrhizae negative sample is the sample lacking Radix Glycyrrhizae by adjusting the technology preparation of stomach CHENGQI TANG granule to prepare, and described Radix Glycyrrhizae negative sample solution is obtained by the method identical with Radix Glycyrrhizae need testing solution.
The detection method of 13. tune stomach CHENGQI TANG granules according to claim 12, wherein, gets described Radix Glycyrrhizae negative sample 5g.
The detection method of 14. tune stomach CHENGQI TANG granules according to claim 1, wherein, in step 2, the content of beary metal≤25ppm recorded.
The detection method of 15. tune stomach CHENGQI TANG granules according to claim 1, wherein, in step 3, described organo-chlorine pesticide is benzene hexachloride, D.D.T. (dichloro-diphenyl-trichloroethane) and pentachloronitrobenzene, the content≤0.20ppm of described benzene hexachloride; Content≤the 0.20ppm of described D.D.T. (dichloro-diphenyl-trichloroethane), the content≤0.10ppm of described pentachloronitrobenzene.
The detection method of 16. tune stomach CHENGQI TANG granules according to claim 1, wherein, described step 6 is undertaken by the method comprised the following steps:
Prepare testing sample solution, pass through high effective liquid chromatography for measuring;
Take octadecylsilane chemically bonded silica as filling agent;
Take methyl alcohol as mobile phase A, 0.1 volume % phosphoric acid is Mobile phase B, and the volume ratio of mobile phase A and Mobile phase B is 80:20; Determined wavelength is 254nm, and number of theoretical plate calculates should be not less than 3000 by archen peak;
Described testing sample solution is obtained by the method that comprises the following steps: get described tune stomach CHENGQI TANG granule and reference substance makes need testing solution and reference substance solution respectively, and described reference substance comprises archen reference substance and/or Chrysophanol reference substance;
Wherein, described need testing solution is obtained by the method comprised the following steps: get described tune stomach CHENGQI TANG granule 0.5 ~ 3.0g, accurately weighed, put in tool plug conical flask, add methanol solution 10 ~ 30ml, close plug, weighed weight, ultrasonic process 15 ~ 35 minutes, cooling, weighed weight again, supply the weight of less loss with methyl alcohol, shake up, filter, get subsequent filtrate, to obtain final product;
Described reference substance solution is obtained by the method comprised the following steps: get reference substance appropriate, adds methanol solution and makes the solution of 1ml containing 5 ~ 20 μ g reference substances.
The detection method of 17. tune stomach CHENGQI TANG granules according to any one of claim 1 to 16, wherein, in the preparation method of the described need testing solution in described step 4 or step 6, gets described tune stomach CHENGQI TANG granule 1.0g; Add methanol solution 25ml; Ultrasonic process 20 minutes.
18. the detection method of the tune stomach CHENGQI TANG granule according to any one of claim 1 to 16, wherein, in the preparation method of the described reference substance solution in described step 4 or step 6, get reference substance appropriate, add methanol solution and make the solution of 1ml containing the reference substance of 10 μ g.
The detection method of 19. tune stomach CHENGQI TANG granules according to any one of claim 1 to 16, wherein, in the preparation method of the described control medicinal material solution in described step 4, adds methyl alcohol 25ml; Ultrasonic process 20 minutes.
The detection method of 20. tune stomach CHENGQI TANG granules according to any one of claim 1 to 16, wherein, mass percentage content >=33.9% of extract in described step 5.
The detection method of 21. tune stomach CHENGQI TANG granules according to any one of claim 1 to 16, wherein, similarity >=0.90 of test sample finger-print and reference substance finger-print.
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| 陈修园.调胃承气汤.《陈修园医学全书》.山西科学技术出版社,2011,(第1版),第733页,尤其是第733页右栏第14-17行. * |
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