CN106668111A - Rhizoma atractylodis macrocephalae formula granule preparation and quality standard identification detection method thereof - Google Patents
Rhizoma atractylodis macrocephalae formula granule preparation and quality standard identification detection method thereof Download PDFInfo
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/28—Asteraceae or Compositae (Aster or Sunflower family), e.g. chamomile, feverfew, yarrow or echinacea
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Abstract
The invention discloses a rhizoma atractylodis macrocephalae formula granule preparation and a quality standard identification detection method thereof. The rhizoma atractylodis macrocephalae formula granule preparation adopts rhizoma atractylodis macrocephalae or medicinal slices thereof as raw materials, and is prepared through the following steps of adding 1500g of rhizoma atractylodis macrocephalae into water with the mass being 8 to 10 times of the mass of the rhizoma atractylodis macrocephalae, decocting for two times, controlling the decoction time for 1 to 1.5 hours every time, filtering, combining filtrate, vacuum concentrating until the filtrate has the relative density ranging from 1.08 to 1.12 under a condition with the temperature being 60 DEG C, adding an auxiliary material, controlling the adding quantity of the auxiliary material to be 20 to 25 percent of the mass of the rhizoma atractylodis macrocephalae, uniformly mixing, filtering, spray drying, controlling the range of extraction amount ranging from 31.5 percent to 42.7 percent, then adding an appropriate amount of dextrin, uniformly mixing, carrying out granulation, and preparing to obtain 1000g of rhizoma atractylodis macrocephalae formula granule preparation. By adopting the processes such as extraction, evaporation, concentration and the like, the prepared rhizoma atractylodis macrocephalae formula granule preparation has a good medicinal efficacy, preferably reserves atractylenolide effective constituents in the preparation, has the efficacies on strengthening the spleen and stomach, and invigorating qi and moisturizing the lung, and is convenient to carry, store and use.
Description
Technical field：
The invention belongs to Chinese medicine is prepared and identification and detection technical field, more particularly to a kind of white atractylodes rhizome dispensing granule preparation and its matter
Amount standard identification and detection method.
Background technology：
The Rhizoma Atractylodis Macrocephalae,《Chinese Pharmacopoeia》Described in, it has a tonifying the spleen and stomach, effect of lung benefiting gas, for weakness of the spleen and stomach, anorexia and loose stool,
Shortness of breath is coughed, lassitude of the limbs and weakness.The Rhizoma Atractylodis Macrocephalae is a kind of conventional tonifying the spleen and stomach of China, lung benefiting gas Chinese herbal medicine, and it is typically the shape of Chinese herbal medicine
Formula is and less with the type of service of Chinese patent medicine such as white atractylodes rhizome dispensing granule preparation using more.
At present, also no on market take Rhizoma Atractylodis Macrocephalae granular preparation as the preparation method and its quality standard for mainly preparing product
Identification and detection method.Production for the Rhizoma Atractylodis Macrocephalae and its preparation brings inconvenience with using, therefore, urgent need will provide a kind of Rhizoma Atractylodis Macrocephalae and match somebody with somebody
The concrete grammar of the quality standard identification and detection of square granule and preparation.
The content of the invention：
The present invention seeks to provide a kind of white atractylodes rhizome dispensing granule preparation and its quality standard identification and detection method.It is with the Rhizoma Atractylodis Macrocephalae or
Its decoction pieces is raw material, and using techniques such as extraction, evaporation and concentration, the white atractylodes rhizome dispensing granule preparation of preparation, medicinal efficacy is good, in preparation
Atractylodes lactone effective ingredient is preferably retained, and it has tonifying the spleen and stomach, effect of lung benefiting gas, and carries, and preserves easy to use.
The present invention discloses a kind of white atractylodes rhizome dispensing granule preparation, and with Rhizoma Atractylodis Macrocephalae and/or atractylodes slice as raw material, it is by such as
Lower section method is prepared, and is that, by Rhizoma Atractylodis Macrocephalae 1500g, addition accounts for the water of Rhizoma Atractylodis Macrocephalae quality 8-10 times, and decoction is secondary, when control is decocted every time
Between 1-1.5 hours, filter, merging filtrate is evaporated to filtrate under 60 DEG C of temperature conditionss, its relative density is 1.08~
1.12, adjuvant is added, the 20-25% that adjuvant addition is Rhizoma Atractylodis Macrocephalae quality is controlled, mix, filtration is spray-dried, and controls paste-forming rate
Scope is 31.5%~42.7%, adds appropriate dextrin, is mixed, and 1000g is made in granulation, and it is light yellow to brown to obtain final product its character
Yellow, gas delicate fragrance, sweet in the mouth, the white atractylodes rhizome dispensing granule of micro-pungent.
It is a further object of the present invention to provide a kind of quality standard identification inspection of white atractylodes rhizome dispensing granule preparation as above
Survey method, including to Rhizoma Atractylodis Macrocephalae, atractylodes slice, the detection of Rhizoma Atractylodis Macrocephalae intermediate quality standard, is characterized in that described to white atractylodes rhizome dispensing
Granular mass identification and detection is included to white atractylodes rhizome dispensing granule granularity, character, moisture content, melting, heavy metal, microbial limit, leaching
Go out the impact of thing and adjuvant to Rhizoma Atractylodis Macrocephalae extractum；The white atractylodes rhizome dispensing granule character for light yellow to brown color, delicate fragrance, sweet in the mouth,
Micro-pungent, bitter, sweet, warm, returns spleen, the granule of stomach；.
The quality standard identification and detection method of white atractylodes rhizome dispensing granule preparation of the present invention, its is described to extractum extraction
Detection, with alcoholic solvent as solvent, is extracted using hot dipping, controls extraction time 1-1.5 hour.
The quality standard identification and detection method of white atractylodes rhizome dispensing granule preparation of the present invention, its Rhizoma Atractylodis Macrocephalae and decoction pieces
Quality control standard is the Rhizoma Atractylodis Macrocephalae. dry rhizome, ethanol of its determination of extractives using mass concentration as 55-60% as solvent, control
Extractum processed is more than or equal to 45%, with liquid-chromatography apparatus to test and analyze instrument.
The quality standard identification and detection method of white atractylodes rhizome dispensing granule preparation of the present invention, its is described to Rhizoma Atractylodis Macrocephalae intermediate
Quality standard detects that, including identifying Rhizoma Atractylodis Macrocephalae intermediate qualitative trait, moisture, melting, leaching analyte detection are described in the Rhizoma Atractylodis Macrocephalae
Mesosome leaches analyte detection to be included determining chromatographic condition and system suitability using liquid chromatogram detector, the system of reference solution
Standby, need testing solution preparation and determination assay method.
The quality standard identification and detection method of white atractylodes rhizome dispensing granule preparation of the present invention, its described heavy metal analysis is
1）Precision weighs white atractylodes rhizome dispensing granule formulation samples 1-2g, and in putting the crucible of blazing constant weight, slowly blazing to complete carbonization, puts
It is cold, plus sulphuric acid 1-2ml, to moistening, after being eliminated to sulphuric acid with low-temperature heat, plus nitric acid 0.5-0.8ml, it is evaporated, steam to nitrogen oxide
After gas is eliminated, cooling, in 500~600 DEG C it is blazing make to be ashed completely, cool down, plus hydrochloric acid 2ml puts and added water after being evaporated in water-bath
15ml, Deca ammonia solution is to the micro- pink of phenolphthalein indicator, then adds pH3.55 acetate buffer 2-3ml, slight fever dissolving
Afterwards, in dislocation nessler colorimetric tube, dilute into 25ml, as need testing solution；2）The reagent for preparing need testing solution is separately taken,
Put after being evaporated in porcelain dish, plus the acetate buffer 2-3ml that pH is 3.5 and water 15-20ml, after slight fever dissolving, dislocation Na Shi ratios
In colour tube, plus the standard lead solution 1-1.5ml of concentration not 10 μ g/ml, then 25-30ml is diluted with water to, as contrast solution；3）
Add each 2-3ml of thioacetamide test solution respectively in contrast solution and need testing solution pipe again, shake up, place 2 minutes, it is same to put white
On paper, from up to down have an X-rayed, the color shown in need testing solution pipe, must not be deeper compared with contrast solution pipe, white atractylodes rhizome dispensing
Content of beary metal in granule is less than 10ppm.
The quality standard identification and detection method of white atractylodes rhizome dispensing granule preparation of the present invention, its described detection to moisture
It is that precision weighs white atractylodes rhizome dispensing granule or Rhizoma Atractylodis Macrocephalae intermediate sample including the water content detection to white atractylodes rhizome dispensing granule or Rhizoma Atractylodis Macrocephalae intermediate
Product 1-2g, tiling is placed in and is dried into the flat weighing botle of constant weight, and it is little that open bottle cover is dried 5 in the case where temperature is for 100~105 DEG C
When, bottle cap is covered, in being transferred to exsiccator, cool down 30 minutes, it is accurately weighed, then be dried 1 hour at the temperature disclosed above, put
It is cold, weigh, to the double difference weighed less than 5mg；According to the weight of less loss, calculate aqueous in test sample
Amount, must not exceed 6.0%.
The quality standard identification and detection method of white atractylodes rhizome dispensing granule preparation of the present invention, its described microbial limit is
The some batch calibratings of white atractylodes rhizome dispensing granule Jing of control, wherein escherichia coli must not be detected, control yeast and mold sum
Respectively ＜ 10 cfu/g total with aerobe.
The quality standard identification and detection method of white atractylodes rhizome dispensing granule preparation of the present invention, its reference solution
Preparation is that precision weighs Rhizoma Atractylodis Macrocephalae control medicinal material 1-1.5g, and in putting round-bottomed flask, add water 50ml, is decocted 1 hour, and filtration, filtrate is used
Ethyl acetate shaking is extracted 4 times, and each 20ml, combining extraction liquid in putting evaporating dish, is evaporated, and residue adds methanol to make dissolving, transfer
To 5ml measuring bottles, plus methanol dilution is to scale, shakes up, and obtains final product.
The quality standard identification and detection method of white atractylodes rhizome dispensing granule preparation of the present invention, its need testing solution
Preparation is that precision weighs this product about 2.0g, and add water 50ml, and ultrasound makes dissolving, is extracted 4 times with ethyl acetate shaking, each 20ml,
Combining extraction liquid, in putting evaporating dish, is evaporated, and residue adds methanol to make dissolving, is transferred to 5ml measuring bottles, plus methanol dilution to scale, shakes
It is even, obtain final product.
In the preparation process of the white atractylodes rhizome dispensing granule preparation of the present invention, preferably control its external production environment and be particularly
The production environment of dry, granulation, packaging etc. controls its environment space temperature for 18~26 DEG C, and humidity is 45~65%.
White atractylodes rhizome dispensing granule formulation products prepared by the inventive method, preparation process is simple is convenient for carrying and uses, and
Using health, the granular preparation product characteristics of the Rhizoma Atractylodis Macrocephalae are prepared：It is bitter, sweet, temperature.Returns spleen, stomach.Function with cure mainly：Invigorating the spleen and benefiting QI, it is dry
Wet diuretic, hidroschesis is antiabortive.For spleen eating less, abdominal distention diarrhea, phlegm retention anti-dazzle nervous, edema, spontaneous perspiration, frequent fetal movement.Per 1g formula
Grain is equivalent to decoction pieces 1.5g.The quality standard identification and detection method of the present invention, for white atractylodes rhizome dispensing granule prepare the technology that provides and
Quality assurance.
Description of the drawings：
Fig. 1, is white atractylodes rhizome dispensing granule HPLC chromatogram；
Fig. 2, is that Fig. 2 is Rhizoma Atractylodis Macrocephalae intermediate compare feature collection of illustrative plates；
Illustrate, 12 features should be presented in the test sample i.e. characteristic spectrum of white atractylodes rhizome dispensing granule prepared by the present invention of the present invention
Peak, and should be corresponding with 12 characteristic peaks in control medicinal material object of reference chromatographic peak；Wherein peak 12 should be with atractylenolide Ⅰ reference substance
Object of reference peak retention time is consistent.
Specific embodiment：
With reference to specific embodiment to the further detailed description of the inventive method.
Embodiment 1, the preparation of white atractylodes rhizome dispensing granule and the identification and detection of quality standard,
Raw material sources, the Rhizoma Atractylodis Macrocephalae of the present invention is the feverfew Rhizoma Atractylodis MacrocephalaeAtractylodesmacrocephalaKoidz. dry root
Granule made by stem.
The preparation method of white atractylodes rhizome dispensing granule of the present invention, is, by Rhizoma Atractylodis Macrocephalae 1500g, to add water 8 times and measure, be i.e. the water of 12000 g, is decocted
Boil secondary, control each decocting time for 1.5 hours, filtration, merging filtrate, the relative density being evaporated at a temperature of 60 DEG C
For 1.08~1.12, add adjuvant dextrin 360g, mix, filtration is spray-dried, control paste-forming rate scope 31.5%~
42.7%, appropriate dextrin is added, mix, 1000g is made in granulation, obtains final product.
The character of white atractylodes rhizome dispensing granule of the present invention, is the light yellow granule to brown color；Gas delicate fragrance, sweet in the mouth, micro-pungent.
The quality standard identification and detection method of white atractylodes rhizome dispensing granule of the present invention, takes the white atractylodes rhizome dispensing granule of present invention preparation
Below sample or this product 1g, finely ground, plus methanol 20ml, supersound process 30 minutes, filtration is claimed to take subsequent filtrate molten as test sample
Liquid.Rhizoma Atractylodis Macrocephalae control medicinal material 0.5g is separately taken, add water 30ml, boiled 20 minutes, filtrate is evaporated, and residue adds methanol 20ml, is made in the same way of
Control medicinal material solution.According to thin layer chromatography（《Chinese Pharmacopoeia》Four general rules 0502 of version in 2015）Test, draws above two molten
The each 1 μ l of liquid, put respectively on same silica gel g thin-layer plate, with chloroform-methanol（6:5）For developing solvent, launch, take out, dry in the air
It is dry, spray with 10% sulphuric acid ethanol, it is heated to spot development at 105 DEG C clear.Test sample is in white atractylodes rhizome dispensing granule chromatograph, with
On the corresponding position of control medicinal material chromatograph principal spot, show the speckle of same color.
Check, granule should be met（《Chinese Pharmacopoeia》Four general rules 0104 of version in 2015）Relevant every regulation under.
Extractum, according to ethanol-soluble extractiveses algoscopy（《Chinese Pharmacopoeia》Four general rules 2201 of version in 2015）Heat under
Leaching method is determined, and takes this product in right amount, finely ground, takes about 2g, accurately weighed, and in putting conical flask with cover, precision adds ethanol 50ml, stands
1 hour, it is heated to reflux 1 hour, extractum must not be less than 6.0%.
Characteristic spectrum, according to high performance liquid chromatography（《Chinese Pharmacopoeia》Four general rules 0512 of version in 2015）Determine.
Chromatographic condition is with system suitability with octadecylsilane chemically bonded silica as filler；With methanol as mobile phase
A, with 0.5% formic acid solution as Mobile phase B, the gradient according to the form below 1 carries out eluting；Column temperature：30℃；Detection wavelength is 313nm.
Table 1
The preparation of reference solution, takes Rhizoma Atractylodis Macrocephalae control medicinal material about 1.5g, and accurately weighed, in putting round-bottomed flask, add water 50ml, decocts
1 hour, filtration, filtrate was extracted 4 times with ethyl acetate shaking, and each 20ml, combining extraction liquid in putting evaporating dish, is evaporated, residue
Plus methanol makes dissolving, 5ml measuring bottles, plus methanol dilution are transferred to scale, are shaken up, obtain final product.
Take atractylodes lactoneAppropriate reference substance, plus methanol make every 1ml containing 10 μ g solution, obtain final product.
Test sample is the preparation of white atractylodes rhizome dispensing granule solution, takes this product i.e. white atractylodes rhizome dispensing granule under content uniformity item, is mixed
It is even, it is finely ground, about 2.0g is taken, accurately weighed, add water 50ml, and ultrasound makes dissolving, is extracted 4 times with ethyl acetate shaking, each 20ml,
Combining extraction liquid, in putting evaporating dish, is evaporated, and residue adds methanol to make dissolving, is transferred to 5ml measuring bottles, plus methanol dilution to scale, shakes
It is even, obtain final product.
Identification and detection method, it is accurate respectively to draw reference solution and each 10 μ l of need testing solution, chromatograph of liquid is injected,
Determine, obtain final product.
Test sample is that 12 characteristic peaks should be presented in white atractylodes rhizome dispensing granule characteristic spectrum, and should be looked for control medicinal material reference
12 characteristic peaks in spectral peak are corresponding；Wherein peak 12 should be consistent with atractylenolide Ⅰ reference substance object of reference peak retention time.
It is determined that the white atractylodes rhizome dispensing granule nature and flavor and return through of the present invention, bitter, sweet, temperature.Returns spleen, stomach.
Function with cure mainly, invigorating the spleen and benefiting QI, eliminate dampness and have diuretic effect, hidroschesis is antiabortive.For spleen eating less, abdominal distention diarrhea, phlegm retention is dizzy
Throb with fear, edema, spontaneous perspiration, frequent fetal movement.
Usage, for formula, is followed the doctor's advice with consumption；Specification, per 1g granules equivalent to decoction pieces 1.5g.
Storage sealing.
Water content detection, shines《Chinese Pharmacopoeia》Four general rules 0832 of version in 2015 are determined, and in four batches pellet moisture meets rule
It is fixed, the results are shown in Table 3.
To Rhizoma Atractylodis Macrocephalae raw material or the quality standard identification and detection of decoction pieces, this Rhizoma Atractylodis Macrocephalae raw material is the light yellow granule to brown color；
Gas delicate fragrance, sweet in the mouth, micro-pungent.
Differentiate, take Rhizoma Atractylodis Macrocephalae raw material or decoction pieces 1g, it is finely ground, plus methanol 20ml, supersound process 30 minutes, filtration, take subsequent filtrate
As need testing solution.Rhizoma Atractylodis Macrocephalae control medicinal material 0.5g is separately taken, add water 30ml, decocted 20 minutes, filtrate is evaporated, and residue adds methanol
20ml, is made in the same way of control medicinal material solution.
With reference to《Medical institutions' Traditional Chinese medicine decocting room management regulation》Chinese crude drug decocting method associative operation code requirement and modern times
Clinical application is accustomed to, and is decocted using marmite.100g medical materials are weighed, is decocted twice, add water first 800ml, soaked 30 minutes, useed force
After fire boils, use slow fire instead and decoct 40 minutes slowly, add water for the second time 600ml, decocts 30 minutes.Merge decoction liquor twice, filtration takes
Filtrate 50ml is evaporated, and with test sample preparation method, makes standard decoction solution.
According to thin layer chromatography（《Chinese Pharmacopoeia》Four general rules 0502 of version in 2015）Test, draws each 1 μ of above-mentioned three kinds of solution
L, puts respectively on same silica gel g thin-layer plate, with chloroform-methanol（6:5）For developing solvent, launch, take out, dry, spray with
10% sulphuric acid ethanol, is heated to spot development clear at 105 DEG C.
As a result：Test sample be Rhizoma Atractylodis Macrocephalae raw material or decoction pieces in chromatograph, in position corresponding with control medicinal material chromatograph principal spot
On, show the speckle of same color, and be consistent with standard decoction chromatograph speckle.
The negative sample 1g that scarce Rhizoma Atractylodis Macrocephalae lacks Rhizoma Atractylodis Macrocephalae raw material or decoction pieces, plus methanol 20ml are taken, negative sample is made in the same way of
Product solution.Simultaneously serviceability test is carried out, investigated the silica gel G plate of different manufacturers, and different such as 6 DEG C and 28 of temperature of expansion
DEG C, the influence factor such as relative humidity such as 51% and 85%, as a result this unfolding condition ruggedness is good, and principal spot is clear.
The granularity quality standard identification and detection of white atractylodes rhizome dispensing granule, granularity is shone《Chinese Pharmacopoeia》Four general rules of version in 2015
0982 second method, double sieve method inspections, four batches of grain graininess meet regulation, the results are shown in Table 2.
The granularity inspection of table 2
2nd, biodiversity standard identification and detection, shines《Chinese Pharmacopoeia》Four general rules 0832 of version in 2015 are determined, four batches of pellet moisture
Meet regulation, the results are shown in Table 3.
The water content detection of table 3
Melting quality standard identification and detection, shines《Chinese Pharmacopoeia》Check under the granule item of four general rules of version in 2015 0104, four
Criticize granule melting and meet regulation, the results are shown in Table 4.
The melting of table 4 is detected
Microbial limit quality standard identification and detection, shines《Chinese Pharmacopoeia》Four general rules 1107 of version in 2015 are checked, the results are shown in Table
5。
The microbial limit of table 5
As a result show, four batches of microorganism particle limits of the present invention meet regulation requirement.
Heavy metal quality standard identification and detection, reference《Chinese Pharmacopoeia》The method inspection of four general rules of version in 2015 0821 second,
This product is taken, described this product is prepared by Rhizoma Atractylodis Macrocephalae and/or atractylodes slice or white atractylodes rhizome dispensing granule or white atractylodes rhizome dispensing granule at this
The detection of the heavy metal of the intermediate in journey etc. can be accurately weighed with following this product as white atractylodes rhizome dispensing granule as follows
This product of about 1g, in putting the crucible of blazing constant weight, slowly blazing to complete carbonization, lets cool, plus sulphuric acid 1ml, makes proper moistening, uses
After low-temperature heat is eliminated to sulphuric acid, plus nitric acid 0.5ml, it is evaporated, after eliminating to nitrogen oxide steam, let cool, it is vehement at 500~600 DEG C
Burning makes to be ashed completely, lets cool, plus hydrochloric acid 2ml, puts and add water after being evaporated in water-bath 15ml, and Deca ammonia solution is to aobvious to phenolphthalein indicator
Pinkish, then it is 3.5,2ml to add acetate buffer to control pH, after slight fever dissolving, in dislocation nessler colorimetric tube, dilute
Into 25ml, as need testing solution.The reagent for preparing need testing solution is separately taken, is put after being evaporated in porcelain dish, plus acetate buffer
It is 3.5,2ml and water 15ml to control pH, after slight fever dissolving, in dislocation nessler colorimetric tube, plus standard lead solution（10μg/ml）1ml,
25ml is diluted with water to again, as contrast solution.Add thioacetamide examination respectively in contrast solution and need testing solution pipe again
The each 2ml of liquid, shakes up, and places 2 minutes, with putting on blank sheet of paper, from up to down has an X-rayed, the color shown in need testing solution pipe with compare
Solution conduit is compared, must not be deeper.The results are shown in Table 6.
The determining heavy metals result of table 6
As a result show, four batches of white atractylodes rhizome dispensing granule content of beary metal are respectively less than 10ppm and close symbol requirement.
Arsenic identification and detection, shines《Chinese Pharmacopoeia》The method inspection of four general rules of version in 2015 0822 first, takes this product Rhizoma Atractylodis Macrocephalae and matches somebody with somebody
Square granule about 1g, it is accurately weighed, in putting crucible, plus 2% ethanolic magnesium nitrate solution 5ml, it is blazing to charcoal with small fire after lighting burning-up
Change, let cool, plus nitric acid 0.5ml, to nitrogen oxide steam it is cleared after, put 500~600 DEG C it is blazing make to be ashed completely, let cool, plus hydrochloric acid
5ml, in moving to A bottles, add water 21ml, then adds potassium iodide test solution 5ml to drip with acid chlorization stannous test solution 5, and in room temperature 10 points are placed
Zhong Hou, plus zinc granule 2g, fill in ready airway C is close on A bottles immediately, and A bottles are put in 25~40 DEG C of water-baths react 45
Minute, take out mercuric bromide reagent paper.Precision measures standard arsenic solution（1μg/ml）2ml, is evaporated, according to test sample processing method from " plus
2% ethanolic magnesium nitrate solution " rises and is operated with method, and the arsenic speckle of generation is compared with standard arsenic speckle, must not be deeper.The results are shown in Table 7.
The arsenic measurement result of table 7
As a result show, four batches of granule arsenic salt contents are respectively less than 2ppm, close and require.
Extractum identification and detection,
Composition in Chinese crude drug can be leached in water or alcohol, and then carry out assay.According to《Chinese Pharmacopoeia》Version in 2015
Specify under one " Rhizoma Atractylodis Macrocephalae " item, without quantitative identification, Jing consulting literatures and grope, it is determined that assay cannot be set up, can temporarily press
Determination of extractives is used as quality control project.Because granule is prepared after decoction pieces are added water to cook, water is selected to be molten
Agent is set up determination of extractives and is had little significance, it is difficult to reflect inherent quality, therefore when selecting solvent, it is also contemplated that adjuvant pair in Chinese medicine preparation
The impact of solvent.Appropriate solvent is selected to carry out determination of extractives, to control the quality of Chinese medicine preparation.
1）Test sample is that white atractylodes rhizome dispensing granule solution manufacturing method is investigated
Extract the investigation of solvent
Take this product i.e. white atractylodes rhizome dispensing granule（Lot number：00315061）In right amount, it is finely ground, about 2g is taken, it is accurately weighed, put the cone of 100ml
In shape bottle, respectively accurate plus ethanol, each 50ml of n-butyl alcohol, close plug, weighed weight, after standing 1 hour, connect reflux condensing tube,
Boiling is heated to, and keeps micro-boiling 1 hour.After letting cool, conical flask, close plug, then weighed weight are removed, respectively with ethanol, positive fourth
Alcohol supplies the weight of less loss, shakes up, and with filter filtration is dried, precision measures filtrate 25ml, puts the evaporating dish being dried to constant weight
In, after being evaporated in water-bath, in 105 DEG C of dryings 3 hours, put in exsiccator and cool down 30 minutes, rapid accurately weighed weight.Calculate
The content of ethanol-soluble extractiveses in test sample（%）.
Extractum extracts solvent measurement result, and extraction solvent is ethanol, n-butyl alcohol, and extractum % is respectively 10.79%,
1.13%；As a result show, different solvents affect larger to the extraction ratio of extractum, because mainly containing volatile oil, flavone in the medical material
Constituents, in ethanol dissolubility is higher for above composition, and ethanol is less as solvent, toxicity is extracted, and considers, therefore selects
Ethanol is extraction solvent.
The investigation of extracting mode,
Cold-maceration takes this product（Lot number：00315061）In right amount, it is finely ground, about 2g is taken, it is accurately weighed, in putting the conical flask of 100ml, essence
Close plus ethanol 50ml, close plug, merceration constantly shakes in first 6 hours, then stands 18 hours, is filtered rapidly with filter is dried, accurate
Subsequent filtrate 10ml is measured, is put and be dried into the evaporating dish of constant weight, after being evaporated in water-bath, in 105 DEG C of dryings 3 hours, put dry
Cool down 30 minutes in dry device, rapid accurately weighed weight.Calculate the content of ethanol-soluble extractiveses in test sample（%）.
Hot dipping takes this product（Lot number：00315061）In right amount, it is finely ground, about 2g is taken, it is accurately weighed, put the conical flask of 100ml
In, precision adds ethanol 50ml, and close plug, weighed weight after standing 1 hour, connects reflux condensing tube, is heated to boiling, and keeps
Micro-boiling 1 hour.After letting cool, conical flask, close plug, then weighed weight are removed, with ethanol the weight of less loss is supplied, shaken up, use drying
Filter is filtered, and precision measures filtrate 25ml, is put and be dried into the evaporating dish of constant weight, after being evaporated in water-bath, in 105 DEG C of dryings
3 hours, put in exsiccator and cool down 30 minutes, rapid accurately weighed weight.Calculate the content of ethanol-soluble extractiveses in test sample
（%）.Extractum extracting mode measurement result is, extracting mode, hot dipping, extractum（%）10.65%.Cold-maceration, 2.18%.Knot
Fruit shows that different extracting mode extraction ratios affect larger, consider, and select hot dipping.
The investigation of extraction time,
Take this product（Lot number：00315061）In right amount, it is finely ground, about 2g is taken, accurately weighed, in putting the conical flask of 100ml, precision adds second
Alcohol 50ml, close plug, weighed weight after standing 1 hour, connects reflux condensing tube, is heated to boiling, keeps micro-boiling 0.5 little respectively
When, 1 hour, 1.5 hours.After letting cool, conical flask, close plug, then weighed weight are removed, with ethanol the weight of less loss are supplied, shaken up,
With filter filtration is dried, precision measures filtrate 25ml, puts and be dried into the evaporating dish of constant weight, after being evaporated in water-bath, in 105
DEG C drying 3 hours, puts in exsiccator and cools down 30 minutes, rapid accurately weighed weight.Calculate ethanol-soluble extractiveses in test sample
Content（%）.
Extractum extraction time measurement result, 0.5 hour extraction time, extractum（%）For 9.49%；Extraction time 1 is little
When, extractum（%）For 10.63%；1.5 hours extraction times, extractum（%）For 10.26%.As a result show, be heated to reflux 1 little
When, you can extract complete.
Impact of the adjuvant to determination of extractives,
The adjuvant that white atractylodes rhizome dispensing granule is added is dextrin, is to investigate whether adjuvant has an impact to measurement result, takes dextrin about 1.0g,
Accurately weighed, in putting the conical flask of 100ml, precision adds ethanol 50ml, close plug, weighed weight after standing 1 hour, to connect backflow
Condensing tube, is heated to boiling, and keeps micro-boiling 1 hour.After letting cool, conical flask, close plug, then weighed weight are removed, mended with ethanol
The weight of sufficient less loss, shakes up, and with filter filtration is dried, precision measures filtrate 25ml, put be dried into the evaporating dish of constant weight,
After being evaporated in water-bath, in 105 DEG C of dryings 3 hours, put in exsiccator and cool down 30 minutes, rapid accurately weighed weight.Calculate for examination
The content of ethanol-soluble extractiveses in product（%）.As a result dextrin is 0.76%；As a result, dextrin does not dissolve in ethanol, and extract content is relatively low,
It is little to granule determination influences, therefore the impact of adjuvant is not considered further that during determination of extractives.
Primarily determining that for analyte detection is leached,
Take this product i.e. white atractylodes rhizome dispensing granule appropriate, it is finely ground, about 2g is taken, accurately weighed, in putting the conical flask of 100ml, precision adds second
Alcohol 50ml, close plug, weighed weight after standing 1 hour, connects reflux condensing tube, is heated to boiling, and keeps micro-boiling 1 hour.Put
After cold, conical flask, close plug, then weighed weight are removed, with ethanol the weight of less loss is supplied, shaken up, it is accurate with filter filtration is dried
Filtrate 25ml is measured, is put and be dried into the evaporating dish of constant weight, after being evaporated in water-bath, in 105 DEG C of dryings 3 hours, put drying
Cool down 30 minutes in device, rapid accurately weighed weight.Calculate the content of ethanol-soluble extractiveses in test sample（%）.Determine in four batches
The content of extractum, the results are shown in Table 8 in test agent.
8 four batches of pilot scale determination of extractives results of table
Conclusion：Tetra- batches of different decoction pieces of Jing carry out pilot scale checking, determine ethanol-soluble extractiveses, it is contemplated that in actual production process
Various influence factors etc., determine that this product ethanol-soluble extractiveses must not be less than 6.0%.
Chromatographic condition is with system suitability with octadecylsilane chemically bonded silica as filler；With methanol as mobile phase
A, with 0.5% formic acid solution as Mobile phase B, the gradient according to the form below carries out eluting；Column temperature：30℃；Detection wavelength is 313nm.
The preparation of reference solution takes Rhizoma Atractylodis Macrocephalae control medicinal material about 1.5g, accurately weighed, and in putting round-bottomed flask, add water 50ml, decocts
1 hour, filtration, filtrate was extracted 4 times with ethyl acetate shaking, and each 20ml, combining extraction liquid in putting evaporating dish, is evaporated, residue
Plus methanol makes dissolving, 5ml measuring bottles, plus methanol dilution are transferred to scale, are shaken up, obtain final product.
Take atractylodes lactoneAppropriate reference substance, plus methanol make every 1ml containing 10 μ g solution, obtain final product.
The preparation of need testing solution takes this product under content uniformity item, mixes, finely ground, takes about 2.0g, accurately weighed, adds water
50ml, ultrasound makes dissolving, is extracted 4 times with ethyl acetate shaking, and each 20ml, combining extraction liquid in putting evaporating dish, is evaporated, residual
Slag adds methanol to make dissolving, is transferred to 5ml measuring bottles, plus methanol dilution to scale, shakes up, and obtains final product.
Algoscopy is accurate respectively to draw reference solution and each 10 μ l of need testing solution, injects chromatograph of liquid, determines, i.e.,
White atractylodes rhizome dispensing granule HPLC chromatogram.
Embodiment 2
The quality standard identification and detection of atractylodes slice, test sample described in the present embodiment is atractylodes slice.I.e. following quality standards
Testing and appraisal done for atractylodes slice.
【Process】By the feverfew Rhizoma Atractylodis MacrocephalaeAtractylodes macrocephalaKoidz. dry rhizome, except roguing
Matter, cleans, and runs through, and cuts sheet, is dried.
This product is removed should be met《Chinese Pharmacopoeia》Relevant every regulation under " Rhizoma Atractylodis Macrocephalae " the decoction pieces item of page 103 of version one in 2015
Outside, should also conform to following provisions：
【Extractum】According to ethanol-soluble extractiveses algoscopy（《Chinese Pharmacopoeia》Four general rules 2201 of version in 2015）Hot dipping under
Determine, use 60% ethanol as solvent, extractum to be less than 35.0%.
【Characteristic spectrum】According to high performance liquid chromatography（《Chinese Pharmacopoeia》Four general rules 0512 of version in 2015）Determine.
Chromatographic condition is with system suitability with octadecylsilane chemically bonded silica as filler；With methanol as mobile phase
A, with 0.5% formic acid solution as Mobile phase B, the gradient according to the form below carries out eluting；Column temperature：30℃；Detection wavelength is 313nm.
The preparation of reference solution, takes Rhizoma Atractylodis Macrocephalae control medicinal material about 1.5g, and accurately weighed, in putting round-bottomed flask, add water 50ml,
Decoct 1 hour, filtration, filtrate is extracted 4 times with ethyl acetate shaking, and each 20ml, combining extraction liquid in putting evaporating dish, is evaporated,
Residue adds methanol to make dissolving, is transferred to 5ml measuring bottles, plus methanol dilution to scale, shakes up, and obtains final product.
Take atractylodes lactoneAppropriate reference substance, plus methanol make every 1ml containing 10 μ g solution, obtain final product.
The preparation of need testing solution takes atractylodes slice（Cross No. three sieves）About 1.5g, accurately weighed, add water 50ml, and ultrasound makes molten
Solution, is extracted 4 times with ethyl acetate shaking, and each 20ml, combining extraction liquid in putting evaporating dish, is evaporated, and it is molten that residue adds methanol to make
Solution, is transferred to 5ml measuring bottles, plus methanol dilution to scale, shakes up, and obtains final product.
Algoscopy is accurate respectively to draw reference solution and each 10 μ l of need testing solution, injects chromatograph of liquid, determines, i.e.,
.
12 characteristic peaks should be presented in test sample characteristic spectrum, and should be with 12 spies in control medicinal material object of reference chromatographic peak
Levy peak corresponding；Wherein peak 12 should be consistent with atractylenolide Ⅰ reference substance object of reference peak retention time.
Embodiment 3
The quality standard identification and detection of intermediate, test sample described in the present embodiment is intermediate.The inspection of i.e. following quality standards
It is for intermediate to survey identification.
【Character】This product is the light yellow loose powder to brown color；Gas delicate fragrance, sweet in the mouth, micro-pungent.
【Differentiate】This product 0.5g is taken, it is finely ground, plus methanol 20ml, supersound process 30 minutes, filtration, subsequent filtrate is taken as examination
Product solution.Rhizoma Atractylodis Macrocephalae control medicinal material 0.5g is separately taken, add water 30ml, boiled 20 minutes, filtrate is evaporated, residue adds methanol 20ml, same to method
Make control medicinal material solution.According to thin layer chromatography（《Chinese Pharmacopoeia》Four general rules 0502 of version in 2015）Test, draws comparison medicine
The μ l of material solution 1, the μ l of need testing solution 1~2 are put respectively on same silica gel g thin-layer plate, with chloroform-methanol（6:5）For exhibition
Agent is opened, is launched, taken out, dried, sprayed with 10% sulphuric acid ethanol, be heated to spot development at 105 DEG C clear.In test sample chromatograph,
On position corresponding with control medicinal material chromatograph principal spot, show the speckle of same color.
Detection,
Moisture, according to aquametry（《Chinese Pharmacopoeia》Version general rule 0832 in 2015）Second method is determined, and takes this product 2g, and precision claims
Fixed, tiling is placed in and is dried into the flat weighing botle of constant weight, and open bottle cover covers bottle cap in 100~105 DEG C of dryings 5 hours,
In being transferred to exsiccator, let cool 30 minutes, it is accurately weighed, then be dried 1 hour in said temperature, let cool, weigh, it is extremely double
The difference weighed is less than till 5mg.According to the weight of less loss, the water content calculated in test sample must not exceed 6.0%.
Melting, takes this product 1g, plus hot water 200ml, stirs 5 minutes, observes immediately.Should all dissolve, there must not be foreign body
And breeze.
【Extractum】According to ethanol-soluble extractiveses algoscopy（《Chinese Pharmacopoeia》Four general rules 2201 of version in 2015）Heat under
Leaching method is determined, and takes this product in right amount, finely ground, takes about 2g, accurately weighed, and in putting conical flask with cover, precision adds ethanol 50ml, stands
1 hour, it is heated to reflux 1 hour, extractum must not be less than 8.0%.
【Characteristic spectrum】According to high performance liquid chromatography（《Chinese Pharmacopoeia》Four general rules 0512 of version in 2015）Determine.
Chromatographic condition is with system suitability with octadecylsilane chemically bonded silica as filler；With methanol as mobile phase
A, with 0.5% formic acid solution as Mobile phase B, the gradient according to the form below carries out eluting；Column temperature：30℃；Detection wavelength is 313nm.
The preparation of reference solution takes Rhizoma Atractylodis Macrocephalae control medicinal material about 1.5g, accurately weighed, and in putting round-bottomed flask, add water 50ml,
Decoct 1 hour, filtration, filtrate is extracted 4 times with ethyl acetate shaking, and each 20ml, combining extraction liquid in putting evaporating dish, is evaporated,
Residue adds methanol to make dissolving, is transferred to 5ml measuring bottles, plus methanol dilution to scale, shakes up, and obtains final product.
Take atractylodes lactoneAppropriate reference substance, plus methanol make every 1ml containing 10 μ g solution, obtain final product.
The preparation of need testing solution takes this product about 2.0g, and accurately weighed, add water 50ml, and ultrasound makes dissolving, uses ethyl acetate
Shaking is extracted 4 times, and each 20ml, combining extraction liquid in putting evaporating dish, is evaporated, and residue adds methanol to make dissolving, is transferred to 5ml amounts
Bottle, plus methanol dilution is to scale, shakes up, and obtains final product.
Algoscopy, it is accurate respectively to draw reference solution and each 10 μ l of need testing solution, chromatograph of liquid is injected, determine,
Obtain final product.12 characteristic peaks should be presented in test sample characteristic spectrum, and should be with 12 features in control medicinal material object of reference chromatographic peak
Peak is corresponding；Wherein peak 12 should be consistent with atractylenolide Ⅰ reference substance object of reference peak retention time.
Claims (10)
1. a kind of white atractylodes rhizome dispensing granule preparation, with Rhizoma Atractylodis Macrocephalae and/or atractylodes slice as raw material, is characterized in that making as follows
It is standby to obtain, it is that, by Rhizoma Atractylodis Macrocephalae 1500g, addition accounts for the water of Rhizoma Atractylodis Macrocephalae quality 8-10 times, decoct secondary, each decocting time 1-1.5 of control
Hour, filter, merging filtrate, filtrate is evaporated under 60 DEG C of temperature conditionss, its relative density is 1.08~1.12, is added
Adjuvant, controls the 20-25% that adjuvant addition is Rhizoma Atractylodis Macrocephalae quality, mixes, and filtration is spray-dried, and controlling paste-forming rate scope is
31.5%~42.7%, add appropriate dextrin, mix, granulation, make 1000g, obtain final product its character be it is light yellow to brown color,
Gas delicate fragrance, sweet in the mouth, the white atractylodes rhizome dispensing granule of micro-pungent.
2. a kind of quality standard identification and detection method of white atractylodes rhizome dispensing granule preparation as claimed in claim 1, including to the Rhizoma Atractylodis Macrocephalae
Medical material, atractylodes slice, the detection of Rhizoma Atractylodis Macrocephalae intermediate quality standard, is characterized in that described to white atractylodes rhizome dispensing granule Quality Identification detection bag
Include and white atractylodes rhizome dispensing granule granularity, character, moisture content, melting, heavy metal, microbial limit, extractum and adjuvant are soaked to the Rhizoma Atractylodis Macrocephalae
Go out the impact of thing；The white atractylodes rhizome dispensing granule character for light yellow to brown color, delicate fragrance, sweet in the mouth, micro-pungent, bitter, sweet, warm, returns spleen,
The granule of stomach.
3. the quality standard identification and detection method of white atractylodes rhizome dispensing granule preparation according to claim 2, is characterized in that described
Extractum is extracted and is detected, with alcoholic solvent as solvent, extracted using hot dipping, control extraction time 1-1.5 hour.
4. the quality standard identification and detection method of white atractylodes rhizome dispensing granule preparation according to claim 2, is characterized in that the Rhizoma Atractylodis Macrocephalae
The quality control standard of medical material and decoction pieces be the Rhizoma Atractylodis Macrocephalae. dry rhizome, second of its determination of extractives with mass concentration as 55-60%
Used as solvent, control extractum is more than or equal to 45% to alcohol, with liquid-chromatography apparatus to test and analyze instrument.
5. the quality standard identification and detection method of white atractylodes rhizome dispensing granule preparation according to claim 2, is characterized in that described
To Rhizoma Atractylodis Macrocephalae intermediate quality standard detect, including to Rhizoma Atractylodis Macrocephalae intermediate qualitative trait identify, moisture, melting, leach analyte detection,
The analyte detection that leaches to Rhizoma Atractylodis Macrocephalae intermediate is included determining chromatographic condition and system suitability using liquid chromatogram detector, is joined
The preparation of preparation, need testing solution according to thing solution and determination assay method.
6. the quality standard identification and detection method of white atractylodes rhizome dispensing granule preparation according to claim 2, is characterized in that described
Heavy metal analysis are 1）Precision weighs white atractylodes rhizome dispensing granule formulation samples 1-2g, slowly blazing in putting the crucible of blazing constant weight
To complete carbonization, let cool, plus sulphuric acid 1-2ml, to moistening, after being eliminated to sulphuric acid with low-temperature heat, plus nitric acid 0.5-0.8ml, steam
It is dry, after eliminating to nitrogen oxide steam, cooling, in 500~600 DEG C it is blazing make to be ashed completely, cool down, plus hydrochloric acid 2ml, put in water-bath
Add water 15ml after being evaporated, and Deca ammonia solution is to the micro- pink of phenolphthalein indicator, then adds pH3.55 acetate buffer 2-
3ml, slight fever dissolving after, in dislocation nessler colorimetric tube, dilute into 25ml, as need testing solution；2）Preparation is separately taken for examination
The reagent of product solution, puts after being evaporated in porcelain dish, plus the acetate buffer 2-3ml that pH is 3.5 and water 15-20ml, slight fever dissolving
Afterwards, in dislocation nessler colorimetric tube, plus the standard lead solution 1-1.5ml of concentration not 10 μ g/ml, then 25-30ml is diluted with water to, make
For contrast solution；3）Add each 2-3ml of thioacetamide test solution respectively in contrast solution and need testing solution pipe again, shake up, put
Put 2 minutes, with putting on blank sheet of paper, from up to down have an X-rayed, the color shown in need testing solution pipe, must not compared with contrast solution pipe
Deeper, the content of beary metal in white atractylodes rhizome dispensing granule is less than 10ppm.
7. the quality standard identification and detection method of white atractylodes rhizome dispensing granule preparation according to claim 2, is characterized in that described
Include the water content detection to white atractylodes rhizome dispensing granule or Rhizoma Atractylodis Macrocephalae intermediate to the detection of moisture, be precision weigh white atractylodes rhizome dispensing granule or
Rhizoma Atractylodis Macrocephalae intermediate sample 1-2g, tiling is placed in and is dried into the flat weighing botle of constant weight, and open bottle cover is 100~105 in temperature
It is dried 5 hours at DEG C, bottle cap is covered, in being transferred to exsiccator, cools down 30 minutes, it is accurately weighed, then do at the temperature disclosed above
Dry 1 hour, let cool, weigh, to the double difference weighed less than 5mg；According to the weight of less loss, test sample is calculated
In water content, must not exceed 6.0%.
8. the quality standard identification and detection method of white atractylodes rhizome dispensing granule preparation according to claim 2, is characterized in that described
Microbial limit is some batch calibratings of white atractylodes rhizome dispensing granule Jing of control, and wherein escherichia coli must not be detected, and control mycete
With yeast sum and the total respectively cfu/g of ＜ 10 of aerobe.
9. the quality standard identification and detection method of white atractylodes rhizome dispensing granule preparation according to claim 4, is characterized in that described
The preparation of reference solution is that precision weighs Rhizoma Atractylodis Macrocephalae control medicinal material 1-1.5g, and in putting round-bottomed flask, add water 50ml, is decocted 1 hour,
Filtration, filtrate is extracted 4 times with ethyl acetate shaking, and each 20ml, combining extraction liquid in putting evaporating dish, is evaporated, and residue adds methanol
Dissolving is made, 5ml measuring bottles, plus methanol dilution is transferred to scale, is shaken up, obtained final product.
10. the quality standard identification and detection method of white atractylodes rhizome dispensing granule preparation according to claim 4, is characterized in that described
The preparation of need testing solution is that precision weighs this product about 2.0g, and add water 50ml, and ultrasound makes dissolving, and with ethyl acetate shaking 4 are extracted
Secondary, each 20ml, combining extraction liquid in putting evaporating dish, is evaporated, and residue adds methanol to make dissolving, is transferred to 5ml measuring bottles, plus methanol
Scale is diluted to, is shaken up, obtained final product.
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| CN113552271A (en) * | 2021-07-30 | 2021-10-26 | 湖南新汇制药股份有限公司 | Quality control method of acanthopanax standard decoction |
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