CN107198719A - The preparation method and method of quality control of canopy scattered seed - Google Patents
The preparation method and method of quality control of canopy scattered seed Download PDFInfo
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- A61K36/48—Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
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- A61K36/53—Lamiaceae or Labiatae (Mint family), e.g. thyme, rosemary or lavender
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Abstract
The present invention relates to a kind of preparation method of canopy scattered seed, specially Chinese ephedra is taken by formula, fry semen armeniacae amarae, roasted perilla fruit, dried orange peel, honey-fried CORTEX MORI, Poria cocos and honey-fried licorice root, then add water to cook, decoction liquor be collected by filtration, then vacuum-concentrcted to relative density be 1.12~1.18 concentrate, dextrin and lactose are added into concentrate again, as substrate, concentrate, fluidized drying plasmid are sprayed into, granularity is screened in the particle of 16 60 mesh, canopy scattered seed is obtained；This method prepares the destruction that canopy scattered seed is avoided that active ingredient, it is ensured that the curative effect of medicine；The invention also discloses the method for quality control of canopy scattered seed, quality control to canopy scattered seed is reached by the content assaying method to multi-target ingredient ephedrine hydrochloride in canopy scattered seed, pseudoephedrine hydrochloride, liquiritin, aurantiamarin, Rosmarinic acid, a kind of detection means is provided for the quality control of canopy powder.
Description
Technical field
The invention belongs to pharmaceutical preparation and field of quality control, it is related to the preparation method of canopy scattered seed, further relates to
Canopy powder granular mass control method.
Background technology
Canopy powder comes from《The formulary of peaceful benevolent dispensary》, canopy powder has diffusing lung, relieving exterior syndrome, the function of expelling phlegm and arresting coughing；Cure mainly lung
Feel cold-evil, cough with dyspnea, chest diaphragm dysphoria, spasm of nape and back, low voice speaking nasal obstruction, Light-headedness, mental disorder is unfavorable, sips sound.We's collection
, all medicine phases 5 make exterior cold solution, lung qi a surname to the medicine of lung channel, and sputum is breathed with cough flat, and all diseases of lung system are all removed, therefore claim " canopy
Dissipate ".Using Chinese ephedra as monarch in side, relieving the exterior syndrome with drugs pungent in flavor and warm in property is freeinged lung and relieving asthma with cold-dispelling.Minister is with perillaseed, pungent fragrant lowering the adverse-rising QI to resolve phlegm, and almond is worked hard
Sharp lung qi, expelling phlegm and arresting coughing drop in temperature, expectorant cough suppressant and anti-asthmatic, two medicines jointly.Adjutant dried orange peel pungent-warm, eliminating dampness and eliminating phlegm, regulating qi-flowing for activating stagnancy, " gas
Suitable then phlegm disappears "；The root bark of white mulberry is sweet cold, and purging the lung of pathogenic fire profit level is breathed heavily；Poria cocos invigorating the spleen excreting dampness, prevents the source of producing phlegm；The common clearing damp dissolving phlegm of three medicines.
Radix glycyrrhizae is to make coordinating the drug actions of a prescription.All medicine compatibilities, inducing diaphoresis is used in combination with resolving sputum, and phlegm wet must disappear, and exterior cold must dissipate, all card self-healing.
Classics recipe standard particle copies the decoction pattern of traditional Chinese medicine decoction, has both retained the spy of traditional decoction active ingredient
Point, turn avoid Chinese patent drug be difficult to disease plus-minus and traditional decoction decoct, it is inconvenient to carry the problem of.The exploitation of the kind, can shape
Into the clinical prescripting mode of " based on classical prescription standard particle, supplemented by single granule, being added and subtracted with disease ", modern clinic use is met
Medicine demand.The exploitation of this product can solve can not decocting altogether for single granule presence and wait the problem of disputing on, and give full play to tradition
The advantage of the compatibility of medicines in a prescription, reaches the effect of attenuation synergistic, particularly important.Composite powdered extracts have not only passed on Chinese medicine single formula
The advantage of particle, while it is contemplated that interaction of the medicine materical crude slice in decoction process, it is theoretical to meet the traditional medication of the traditional Chinese medical science, with compared with
Big value.
It is suitable for the clinical compound granular adjusted because China there is no, the Chinese native medicine compound prescription pellet of current international marketing is equal
From Japan, South Korea and China Taiwan.The international market for promoting Chinese herbal granules is opened up in the research of the kind, in promotion
Medicine internationalizes.Therefore, it is necessary in research and development and domestic canopy powder, and the preparation researched and developed to canopy powder must clear and definite quality control side
Method.There is Research Literature report to carry out wherein ephedrine hydrochloride, semen armeniacae amarae to the canopy powder traditional decoction of same prescription but different preparation methods
Glycosides, glycyrrhizic acid, assay (Jin Fengyun, He Zhuying, Zhao Yang, the Liao Wei, beam light justice .HPLC measure canopy powder tradition of liquiritin
Ephedrine hydrochloride, amarogentin, glycyrrhizic acid, the content of liquiritin in decoction and Granules decoction, Chinese patent drug, 2008 years volume 30 the
1 phase), it is another that studies have reported that determining aurantiamarin composition therein, (Zhang Mingchang, Shao Jinming, Peng little Bing, Yuan Shuanxiu, beam light justice are anti-phase
Precious traditional Chinese medical science traditional Chinese medicines during the content of aurantiamarin in high effective liquid chromatography for measuring difference preparation method canopy powder, 2010 volume 21 the 1st
Phase).The above-mentioned quantitatively or qualitatively method reported at present can't efficiently control the quality of canopy scattered seed.
The content of the invention
In view of this, it is an object of the invention to provide a kind of preparation method of canopy scattered seed, this method can fully be sent out
The characteristic of drug matching and the advantage of traditional decoction are waved, active ingredient is remained to greatest extent；The second object of the present invention exists
In the method for quality control for providing canopy scattered seed, this method is the weak point for overcoming existing quality standard supervision, for
Canopy scattered seed provides a kind of detection means of system, by multi-target ingredient ephedrine hydrochloride, salt in canopy scattered seed
Sour pseudoephedrine, liquiritin, aurantiamarin, the content assaying method of Rosmarinic acid reach the quality control to canopy scattered seed.
To reach above-mentioned purpose, the present invention provides following technical scheme：
1st, the preparation method of canopy scattered seed, comprises the following steps：
A, in mass ratio be 1-3：1-3：1-3：1-3：1-3：1-3：1-3：1-3 takes Chinese ephedra, fries semen armeniacae amarae, fries purple perilla respectively
Son, dried orange peel, honey-fried CORTEX MORI, Poria cocos and honey-fried licorice root, the water for then adding 6~12 times equivalent to medicinal material gross mass decoct for the first time
Boil, filtrate is collected by filtration, the water that the dregs of a decoction add 4~10 times equivalent to medicinal material gross mass carries out second of decoction, is collected by filtration
Filtrate, the water that the dregs of a decoction add 3-8 times equivalent to medicinal material gross mass carries out third time decoction, and filtrate is collected by filtration；
B, 3 decoction filtrates of merging, filtration, filter vacuum are concentrated under reduced pressure into the concentration that relative density is 1.12~1.18
Liquid；
C, using the mixture of dextrin and lactose as substrate, spray into concentrate obtained by step b, fluidized drying plasmid, sieve
Select granularity in the particle of 16-60 mesh, obtain canopy scattered seed.
It is preferred that, the Chinese ephedra, the mass ratio for frying semen armeniacae amarae, roasted perilla fruit, dried orange peel, honey-fried CORTEX MORI, Poria cocos and honey-fried licorice root
For 3：3：3：3：3：3：1.5.
It is preferred that, the first time decocting time is 1~3 hour, and second of decocting time is 1~1.5 hour, institute
Third time decocting time is stated for 0.5~1.5 hour.
In step c of the present invention, the mass ratio of the dextrin and lactose is 3:1.
In the present invention, the fluidized drying condition is EAT：80 DEG C, blower fan frequency 35Hz, charging rate 40r
min-1, atomizing pressure 0.1Mpa.
In the present invention, the mixture addition of the dextrin and lactose is 1.12 times of dry cream amount.
2nd, the method for quality control of canopy scattered seed, comprises the following steps：
(1) ephedrine hydrochloride, the measure of pseudoephedrine hydrochloride content：Canopy scattered seed is taken, methanol solution is added after grinding, is surpassed
Sound dissolves, cooling, then adds methanol solution to supply weightlessness, shakes up, and filters, and collects filtrate and obtains canopy powder particulate samples；Hydrochloric acid Chinese ephedra
Alkali, pseudoephedrine hydrochloride standard items methanol solution dissolve, and shake up to obtain standard solution, then by canopy powder particulate samples and mark
Quasi- product solution is detected under following chromatographic condition：Chromatographic column：Length and a diameter of 250mm × 4.6mm, 5 μm of Kromasil
100-5Phenyl；Column temperature：27℃；Sample size：10μl；Flow velocity：1.0ml·min-1；Mobile phase：Acetonitrile and phosphoric acid quality fraction
It is 1: 99 for 0.1% phosphoric acid water volume ratio；Detection wavelength：210nm；
(2) measure of liquiritin, aurantiamarin, rosmarinic acid contents：Take and methanol solution is used after canopy powder particulate abrasive, be made
Then liquiritin, aurantiamarin, Rosmarinic acid standard items are added methanol to dissolve by canopy powder particulate samples, and mark product solution is made, then will
Canopy powder particulate samples and standard solution are detected under following chromatographic condition：Chromatographic column：Length and diameter 250 × 4.6mm, 5 μ
M Thermo Syncronis C18；Column temperature：27℃；Mobile phase：The phosphoric acid water of acetonitrile -0.01%；Sample size：20μl；Flow velocity：
1.0ml·min-1；Mobile phase：Acetonitrile and the phosphoric acid water gradient elution that phosphoric acid quality fraction is 0.1%, 0~12min acetonitrile bodies
Product is than being 18%, and 12~30min acetonitriles volume ratio is 20%, and 30~40min acetonitriles volume ratio is 25%, 40~55min acetonitriles
Volume ratio is 100%；
(3) result judges：Canopy powder particulate samples are in ephedrine hydrochloride, pseudoephedrine hydrochloride, liquiritin, aurantiamarin and fan
Repeatedly appearance meets quality standard at fragrant acidity scale product appearance.
In step (1) of the present invention, canopy powder particulate samples preparation method is：Canopy scattered seed is taken, 3 every gram of China are pressed after grinding
Lid scattered seed adds the methanol solution that the hydrochloric volume fractions of 250ml are 50%, ultrasonic dissolution, cooling, then adds hydrochloric body
Fraction supplies weightlessness for 50% methanol solution, shakes up, and filters, and collects filtrate and obtains canopy powder particulate samples；The methanol is molten
Hydrochloric acid mass fraction is 0.036% in liquid；
Standard solution preparation method is：Ephedrine hydrochloride, pseudoephedrine hydrochloride are weighed respectively, are 50% with volume fraction
Methanol dissolve and dilute, be configured to hydrochloric ephedrine, pseudoephedrine hydrochloride be respectively 20 μ g/ml, 10 μ g/ml solution i.e.
Can.
In step (2) of the present invention, canopy powder particulate samples preparation method is：Canopy scattered seed is taken, by every gram of canopy powder
Grain plus 100ml methanol, the ultrasonic extraction 30min under the conditions of frequency 40kHz, power 240W are taken out, and weightlessness is supplied in cooling,
10000r·min-110min is centrifuged, supernatant is filtered with 0.45 μm of miillpore filter；
Standard solution preparation method is：Liquiritin, aurantiamarin, Rosmarinic acid are weighed respectively, plus methanol dissolving is configured to
Concentration is respectively 0.3733mgml-1、0.0902mg·ml-1And 0.1911mgml-1Solution.Dry cream amount is Chinese medicine through water
Decoct, the lotion being dried to obtain after concentration.
The beneficial effects of the present invention are：The preparation method of canopy scattered seed, this method is conventionally decocted and is made
Compound granular, each flavour of a drug are simply added when more current single granule is taken, and can more give full play to the advantage of drug matching, body
The overall idea of traditional Chinese medicine is showed, new selection is provided for clinical application；Boiling granulating technology is used in preparation technology, will be extracted
The multiple operation such as medicinal extract is mixed with auxiliary material, pelletized, drying, whole grain, are completed in a granulator, improve tradition granulation multimachine combination
Technique drawback, make material complete under cryogenic dry, pelletization, it is to avoid the destruction of active ingredient, it is ensured that medicine
Curative effect.
, can be more fully by multi objective assay the invention also discloses the method for quality control of canopy scattered seed
Ground is evaluated by the quality of canopy scattered seed, it is ensured that the stability of product quality and the validity of clinical application and security.
The present invention has the characteristics of detection means is simple, testing result is accurate, quality surveillance is more comprehensive, can more be adapted to overall Chinese medicine matter
The requirement that amount control is improved.
Brief description of the drawings
In order that the purpose of the present invention, technical scheme and beneficial effect are clearer, the present invention provides drawings described below and carried out
Explanation：
Fig. 1 is ephedrine hydrochloride, pseudoephedrine hydrochloride specificity investigation collection of illustrative plates (A：Solvent；B：Ephedrine hydrochloride；C：Hydrochloric acid
Pseudoephedrine).
Fig. 2 is liquiritin, aurantiamarin, Rosmarinic acid specificity investigation HPLC collection of illustrative plates (A：Liquiritin；B：Aurantiamarin；C：Fan
It is repeatedly fragrant sour).
Embodiment
Below in conjunction with accompanying drawing, the preferred embodiments of the present invention are described in detail.
Embodiment 1
The preparation method of canopy scattered seed, comprises the following steps：
A, take Chinese ephedra 300g, fry semen armeniacae amarae 300g, roasted perilla fruit 300g, dried orange peel 300g, honey-fried CORTEX MORI 300g, Poria cocos
300g, honey-fried licorice root 150g, plus 19.5kg water, decoct extract 2 hours, i.e., one decoct；One decocts the water that the rear dregs of a decoction add 15.6kg, decocts
Extraction 1 hour, i.e., two are boiled to decoct；Two decoct the water that the rear dregs of a decoction add 11.7kg, decoct extraction 1.0 hours, i.e., three and decoct；
B, three decoction filtrates of merging, filtration, filter vacuum are concentrated under reduced pressure into relative density for 1.14~1.15 (60 DEG C)
Concentrate；
C, addition weight ratio are 3:1 dextrin and lactose mixes (mixture addition is 1.12 times of dry cream amount), as
Substrate, sprays into above-mentioned concentrate, and fluidized drying granulation controls EAT：80 DEG C, blower fan frequency 35Hz, charging rate 40r
min-1, atomizing pressure 0.1Mpa, be made granularity 16-60 mesh canopy scattered seed.
Embodiment 2
The preparation method of canopy scattered seed, comprises the following steps：
A, take Chinese ephedra 300g, fry semen armeniacae amarae 300g, roasted perilla fruit 300g, dried orange peel 300g, honey-fried CORTEX MORI 300g, Poria cocos
300g, honey-fried licorice root 150g, plus 23.4kg water, decoct extract 2.5 hours, i.e., one decoct；One decocts the water that the rear dregs of a decoction add 19.5kg,
Extraction 1.5 hours, i.e., two are decocted to decoct；Two decoct the water that the rear dregs of a decoction add 15.6kg, decoct extraction 1 hour, i.e., three and decoct；
B, three decoction filtrates of merging, filtration, filter vacuum are concentrated under reduced pressure into relative density for 1.15~1.16 (60 DEG C)
Concentrate；
C, addition weight ratio are 3:1 dextrin and lactose is mixed, as substrate, sprays into above-mentioned concentrate, fluidized drying system
Grain, controls EAT：80 DEG C, blower fan frequency 35Hz, charging rate 40rmin-1, atomizing pressure 0.1Mpa, be made granularity exist
The canopy scattered seed of 16-60 mesh.
Embodiment 3
The preparation method of canopy scattered seed, comprises the following steps：
A, take Chinese ephedra 300g, fry semen armeniacae amarae 300g, roasted perilla fruit 300g, dried orange peel 300g, honey-fried CORTEX MORI 300g, Poria cocos
300g, honey-fried licorice root 150g, plus 15.6kg water, decoct extract 3 hours, i.e., one decoct；One decocts the water that the rear dregs of a decoction add 11.7kg, decocts
Extraction 1 hour, i.e., two are boiled to decoct；Two decoct the water that the rear dregs of a decoction add 7.8kg, decoct extraction 0.5 hour, i.e., three and decoct；
B, three decoction filtrates of merging, filtration, filter vacuum are concentrated under reduced pressure into relative density for 1.17~1.18 (60 DEG C)
Concentrate；
C, addition weight ratio are 3:1 dextrin and lactose is mixed, as substrate, sprays into above-mentioned concentrate, fluidized drying system
Grain, controls EAT：80 DEG C, blower fan frequency 35Hz, charging rate 40rmin-1, atomizing pressure 0.1Mpa, be made granularity exist
The canopy scattered seed of 16-60 mesh.
Embodiment 4
The preparation method of canopy scattered seed, including step are as follows：
A, take Chinese ephedra 300g, fry semen armeniacae amarae 300g, roasted perilla fruit 300g, dried orange peel 300g, honey-fried CORTEX MORI 300g, Poria cocos
300g, honey-fried licorice root 150g, plus 11.7kg water, decoct extract 1 hour, i.e., one decoct；One decocts the water that the rear dregs of a decoction add 7.8kg, decocts
Extraction 1 hour, i.e., two are boiled to decoct；Two decoct the water that the rear dregs of a decoction add 5.85kg, decoct extraction 1.5 hours, i.e., three and decoct；
B, three decoction filtrates of merging, filtration, filter vacuum are concentrated under reduced pressure into relative density for 1.12~1.13 (60 DEG C)
Concentrate；
C, addition weight ratio are 3:1 dextrin and lactose is mixed, as substrate, sprays into above-mentioned concentrate, fluidized drying system
Grain, controls EAT：80 DEG C, blower fan frequency 35Hz, charging rate 40rmin-1, atomizing pressure 0.1Mpa, be made granularity exist
The canopy scattered seed of 16-60 mesh.
Embodiment 5, canopy powder particle content measuring
Canopy scattered seed prepared by embodiment 1~4 carries out assay, using high performance liquid chromatography, specific steps
It is as follows：
1st, ephedrine hydrochloride, the content assaying method of pseudoephedrine hydrochloride are：
(1) sample, instrument and reagent：
Canopy scattered seed (lot number：15120001、15120002、15120003、16010001、16010002、
16010003rd, 16020001,16020002,16020003,16030001) ephedrine hydrochloride reference substance (Chinese food medicine is examined
Determine research institute, lot number 110749-200714, mass fraction 99.8%), pseudoephedrine hydrochloride reference substance (examine by Chinese food medicine
Determine research institute, lot number 110715-200212, mass fraction 99.9%).
The quaternary gradient pumps (Agilent company of the U.S.) of Agilent 1100 and automatic sampler；Sartorius-BS 124S
Type precision electronic balance (German Sai Duolisi balances Co., Ltd)；KQ2200E types are cleaned by ultrasonic machine (the phase instrument instrument of Shanghai five
Table Co., Ltd)；Ultrasonic washing instrument (KQ3200DE, Kunshan Ultrasonic Instruments Co., Ltd.).
Methanol, second eyeball (U.S. Fisher), triethylamine, di-n-butylamine, phosphoric acid (the limited public affairs of Tianjin Ke Miou chemical reagent
Department)；Water is double distilled water；Remaining reagent is that analysis is pure.
(2) method and result：
The selection of Detection wavelength：Precision weighs ephedrine hydrochloride, pseudoephedrine hydrochloride reference substance 10mg, 5mg, plus methanol and matched somebody with somebody
Ephedrine hydrochloride processed, the μ g/ml of pseudoephedrine hydrochloride 20,10 μ g/ml.Using methanol as blank correction, in the range of 200~400nm
Scanning, determines the maximum absorption wavelength λ of ephedrine hydrochloride, pseudoephedrine hydrochloridemaxFor 210nm.
The determination of chromatographic condition：
Chromatographic column：Length and a diameter of 250mm × 4.6mm, 5 μm of Kromasil 100-5Phenyl；Column temperature：27℃；
Sample size：10μl；Flow velocity：1.0ml·min-1；Mobile phase：(wt) % of acetonitrile -0.1 phosphoric acid waters (containing 0.04 (wt) % triethylamines and
0.02 (wt) % di-n-butylamines) (1: 99).
The preparation of reference substance solution：
Precision weighs ephedrine hydrochloride, pseudoephedrine hydrochloride reference substance in right amount, plus 50% methanol dissolves and diluted, and is matched somebody with somebody
It is made in every ml and distinguishes hydrochloric ephedrine, the μ g of pseudoephedrine hydrochloride 20,10 μ g mixed solutions, shakes up, produce.
The preparation of need testing solution：
Canopy powder standard particle is taken, it is finely ground, fine powder about 0.3g is taken, is put in 25ml measuring bottles, plus 50% methanol solution
(0.036% hydrochloric acid), ultrasonic (500W, 40kHz) processing 30min, taking-up is let cool, plus 50% methanol solution (0.036% hydrochloric acid)
To scale, shake up, centrifuge, take supernatant to filter, take subsequent filtrate, produce.
(3) exclusive Journal of Sex Research
Take canopy powder standard particle sample and scarce Chinese ephedra negative sample, be made need testing solution, lack Chinese ephedra test sample it is molten
Liquid.Three kinds of solution are drawn respectively, according to the chromatographic condition drafted, are injected liquid chromatograph, are recorded chromatogram, seeing Fig. 1, (1- salt is tingle
Yellow alkali peak, 2- pseudoephedrine hydrochlorides peak；A- lacks the canopy powder negative sample of Chinese ephedra, B- ephedrine hydrochlorides, pseudoephedrine hydrochloride pair
According to product, C- canopy powders standard particle).
(4) investigation of linear relationship
Accurate reference substance stock solution of drawing is put in volumetric flask plus methanol constant volume respectively, forms the mixing control of 5 concentration
Product solution, injects liquid chromatograph, records chromatogram, using peak area as ordinate, and the sample size (μ g) of reference substance is abscissa,
By principle of least square method fit equation, standard curve is drawn, ephedrine hydrochloride equation is y=2.157x-2.481, r=
0.9999；Pseudoephedrine hydrochloride equation is y=2.230x+2.485, r=1.0000.As a result show, ephedrine hydrochloride sample size
It is good with respective peaks area linear relation in 31~993 μ g ranges；Pseudoephedrine hydrochloride sample size is in 29~933 μ g ranges
It is interior, it is good with respective peaks area linear relation.
(5) recovery test
Taking this product particle, (ephedrine hydrochloride, pseudoephedrine hydrochloride content are respectively：1.61mg·g-1、0.60mg·g-1)
In right amount, finely ground, precision weighs 9 parts, puts respectively in 25ml measuring bottles, then accurate add mixes reference substance (hydrochloric ephedrine
0.02643mg·ml-1, pseudoephedrine hydrochloride 0.01002mgml-1) in right amount, then add 50% methanol solution (to contain 0.036% salt
Acid) in right amount, need testing solution is prepared by test sample preparation method, according to the chromatographic condition drafted, 10 μ l test samples are drawn respectively
Solution, reference substance solution record chromatogram in liquid chromatograph, calculate average recovery, as a result such as Tables 1 and 2.As a result table
It is bright：Ephedrine hydrochloride, the pseudoephedrine hydrochloride content rate of recovery are good in this method detection canopy powder standard particle, and meeting analysis will
Ask.
Calculation formula is following (similarly hereinafter)：
Table 1, the experiment of ephedrine hydrochloride average recovery
Table 2, the experiment of pseudoephedrine hydrochloride average recovery
(6) precision test
A. repeatability is investigated
Take canopy powder standard particle appropriate, it is finely ground, 6 parts are weighed, is prepared by need testing solution preparation method, peak face is determined
Product, calculates content, investigates result and shows that ephedrine hydrochloride, pseudoephedrine hydrochloride RSD are respectively 0.96%, 0.90%, repeatability
Well.
B. different personnel's precision are investigated
Canopy powder standard particle is taken, by 3 different staff, is prepared respectively for examination by need testing solution preparation method
2 parts of product solution, determines its peak area, calculates content, as a result shows：The precision RSD that personnel change for respectively 0.64%,
1.64%, show that different personnel's precision are good.
C. same date precision is not investigated
Canopy powder standard particle is taken, within different working days, 2 parts, survey are prepared respectively by need testing solution preparation method
Determine peak area, calculate content, as a result same date precision is not investigated, both day to day precision RSD are 1.89%, 3.28%, table
Bright day to day precision is good.
D. different instrument precisions are investigated
Canopy powder standard particle is taken, on different instruments, 2 parts, measure are prepared respectively by need testing solution preparation method
Peak area, calculates content, and as a result different instrument precisions are investigated, the precision RSD that instrument changes is respectively 0.66%,
1.64%, show that precision is good.
(7) investigation of stability
Canopy powder standard particle is taken, need testing solution is prepared by need testing solution preparation method, in different time intervals,
It is accurate respectively to draw 10 μ l, by above-mentioned chromatographic condition, liquid chromatograph is injected, peak area is recorded.As a result show：Need testing solution
It is closed at room temperature to preserve, 24h is deposited, is respectively to ephedrine hydrochloride, pseudoephedrine hydrochloride retention time and peak area RSD
1.49th, 1.86%, have good stability.
(8) ephedrine hydrochloride, the determination of pseudoephedrine hydrochloride content limit
Each batch sample test liquid is prepared by above-mentioned test sample compound method, above method determines 10 batch canopy powder granulated salts
Sour ephedrine, pseudoephedrine hydrochloride content.Obtaining average content is respectively：1.43mg/g、0.54mg/g；Determine ephedrine hydrochloride,
The content limit of pseudoephedrine hydrochloride is respectively：1.14mg/g, 0.43mg/g, the results are shown in Table 3.
Ephedrine hydrochloride, the measurement result of pseudoephedrine hydrochloride content in table 3, different batches canopy scattered seed
2nd, the measure of liquiritin, aurantiamarin, rosmarinic acid contents.
(1) sample, instrument and reagent
Sample：Canopy scattered seed (the same ephedrine hydrochloride of sample, pseudoephedrine hydrochloride content assaying method sample)；Radix glycyrrhizae
Glycosides reference substance (National Institute for Food and Drugs Control, lot number 111610-201106, mass fraction 93.7%), aurantiamarin control
Product (National Institute for Food and Drugs Control, lot number 110796-200310, mass fraction 95.3%), Rosmarinic acid reference substance (in
Food and medicine calibrating research institute of state, lot number 111871-201404, mass fraction 98.6%).
Instrument：The quaternary gradient pumps (Agilent company of the U.S.) of Agilent 1100 and automatic sampler；Sartorius-BS
124S types precision electronic balance (German Sai Duolisi balances Co., Ltd)；KQ2200E types are cleaned by ultrasonic machine (the phase instrument of Shanghai five
Instruments and meters Co., Ltd)；Ultrasonic washing instrument (KQ3200DE, Kunshan Ultrasonic Instruments Co., Ltd.).
Reagent：Methanol, second eyeball (U.S. Fisher), phosphoric acid (Tianjin Ke Miou chemical reagent Co., Ltd)；Water is attached most importance to steaming
Distilled water；Remaining reagent is that analysis is pure.
(2) method and result
The determination of chromatographic condition：Chromatographic column：Thermo Syncronis C18(250 × 4.6mm, 5 μm)；Column temperature：27℃；
Mobile phase：The phosphoric acid water of acetonitrile -0.01%；Sample size：20μl；Flow velocity：1.0ml·min-1；Mobile phase：A (acetonitrile)-B (0.01
(wt) % phosphoric acid waters)；Gradient elution program：0min → 12min → 30min → 40min → 55min, acetonitrile 18% → 20% →
25% → 100% → 100%.
The preparation of reference substance solution：Precision weighs reference substance liquiritin, aurantiamarin, appropriate Rosmarinic acid, put respectively 25ml,
In 100ml, 25ml measuring bottle, plus methanol dissolving and constant volume, shake up, producing reference substance stock solution I, II, III, (concentration is respectively
0.3733mg·ml-1、0.0902mg·ml-1、0.1911mg·ml-1)。
The preparation of need testing solution：Take appropriate test sample finely ground, precision weighs about 0.25g in tool plug triangular pyramidal bottle,
Add 25ml methanol.Weigh, ultrasonic (frequency 40kHz, power 240W) extracts 30min, take out, let cool, mend weight, 10000r
min-110min is centrifuged, subsequent filtrate (0.45 μm) filtration of miillpore filter is used as test liquid.
The selection of Detection wavelength：Precision weighs liquiritin, aurantiamarin, Rosmarinic acid reference substance in right amount, plus methanol prepares sweet
(concentration is respectively 0.3733mgml for careless glycosides, aurantiamarin, Rosmarinic acid-1、0.0902mg·ml-1、0.1911mg·ml-1).In
Scanned in the range of 200~400nm, determine the maximum absorption wavelength λ of liquiritin, aurantiamarin, Rosmarinic acidmaxFor 278nm.
(3) exclusive Journal of Sex Research
Take canopy powder standard particle sample and while lack radix glycyrrhizae, dried orange peel, the negative sample of perilla seed, by drafting sample treatment
Method processing, be prepared into canopy powder standard particle need testing solution, while lack radix glycyrrhizae, dried orange peel, perilla seed negative test sample it is molten
Liquid.Three kinds of solution are taken by chromatographic condition is drafted, 20 μ l are drawn respectively, liquid chromatograph is injected, chromatogram are recorded, seeing Fig. 2, (1- is sweet
Careless glycosides peak, 2- aurantiamarins peak, 3- Rosmarinic acids peak；A- mixed reference substance solutions HPLC schemes, and B- lacks radix glycyrrhizae, dried orange peel, perilla seed medicine
The negative sample of material, C- canopy powder standard particles sample).As a result show, while lacking radix glycyrrhizae, dried orange peel, the negative sample of perilla seed
Solution is noiseless at main peak, and method specificity is good.
(4) range of linearity is investigated
Accurate reference substance stock solution of drawing is put in volumetric flask plus methanol constant volume respectively, forms the mixing control of 5 concentration
Product solution, injects liquid chromatograph, records chromatogram, and with sample size (μ g) for abscissa, peak area is ordinate, draws standard
Curve, the regression equation of liquiritin is calculated by principle of least square method：Y=2375.02x-18.545, correlation coefficient r is
0.99993 (μ g of the range of linearity 0.012~0.598), the regression equation of aurantiamarin：Y=2032.02x-60.016, correlation coefficient r
For 0.99987 (μ g of the range of linearity 0.043~1.442)；The regression equation of Rosmarinic acid：Y=1928.39x-15.077 is related
Coefficient r is 0.99997, (μ g of the range of linearity 0.012~0.458).As a result show, three's linear relationship is good.
(5) recovery test
(concentration is respectively for extracting liquorice glycosides, aurantiamarin, Rosmarinic acid mixed reference substance solution：0.0747mg·ml-1、
0.6045mg·ml-1、0.0573mg·ml-1) add known content particle in (surveyed liquiritin, aurantiamarin, Rosmarinic acid
Content is respectively：0.90mg·ml-1、6.60mg·ml-1、0.64mg·ml-1), prepare test sample by test sample preparation method molten
Liquid, prepares according to need testing solution preparation method, by chromatographic condition is drafted, 20 μ l need testing solutions is drawn respectively and reference substance is molten
Liquid, injects liquid chromatograph, records chromatogram, and calculates average recovery, as a result such as table 4~6.As a result show：This method is examined
Liquiritin, aurantiamarin, the rosmarinic acid contents rate of recovery in canopy powder standard particle is surveyed well, to meet analysis and require.
Table 4, the experiment of liquiritin average recovery
Table 5, the experiment of aurantiamarin average recovery
Table 6, the experiment of Rosmarinic acid average recovery
(6) precision test
A. repeatability is investigated：Take appropriate amount of sample finely ground, weigh 6 parts, need testing solution is prepared by test sample preparation method, point
Its peak area is not determined, content is calculated, and as a result RSD is 0.62%, 0.766%, 0.80%, and repeatability is good.
B. different personnel's precision are investigated
Canopy powder standard particle sample is taken, by 3 different staff, is prepared by need testing solution preparation method for examination
2 parts of product solution, determines its peak area respectively, calculates content, as a result shows：The precision RSD that personnel change is respectively less than 2%, essence
Density is good.
C. same date precision is not investigated
Take canopy powder standard particle sample, within different working days, test sample is prepared by need testing solution preparation method
2 parts of solution, determines its peak area respectively, calculates content, as a result shows：Day to day precision RSD is respectively less than 2%, shows smart in the daytime
Density is good.
D. different instrument precisions are investigated
Canopy powder standard particle is taken, on different instruments, 2 parts, measure are prepared respectively by need testing solution preparation method
Peak area, calculates liquiritin, aurantiamarin, rosmarinic acid contents, and the precision RSD that as a result instrument changes is respectively less than 2%, shows essence
Density is good.
(7) stability test
Canopy powder standard particle is taken, need testing solution is prepared by need testing solution preparation method, respectively at the different time
Interval, precision draws 20 μ l, by above-mentioned chromatographic condition, injects liquid chromatograph, record liquiritin, aurantiamarin, Rosmarinic acid peak
Area.As a result show：Need testing solution is closed at room temperature to be preserved, and 24h is deposited, when retaining liquiritin, aurantiamarin, Rosmarinic acid
Between and peak area variation be respectively less than 2.0%, have good stability.
(8) liquiritin, aurantiamarin, the determination of rosmarinic acid contents limit：
Precision draws liquiritin, aurantiamarin, (concentration is respectively 0.3733mgml to Rosmarinic acid reference substance-1、
0.0902mg·ml-1、0.1911mg·ml-1) and the μ l of need testing solution 20, under above-mentioned condition, liquid chromatograph is injected, is surveyed
It is fixed.
Each batch sample test liquid is prepared by above-mentioned test sample compound method, it is sweet that above method determines 10 batch canopy scattered seeds
Careless glycosides, aurantiamarin, rosmarinic acid contents.It is respectively liquiritin 0.71mg/g, aurantiamarin 6.71mg/g, rosemary to obtain average content
Sour 0.31mg/g；Determine that liquiritin, aurantiamarin, the content limit of Rosmarinic acid are：Liquiritin 0.57mg/g, aurantiamarin
5.37mg/g, Rosmarinic acid 0.25mg/g.It the results are shown in Table 7.
Liquiritin, aurantiamarin, the measurement result of rosmarinic acid contents in table 7, different batches canopy scattered seed
Finally illustrate, preferred embodiment above is merely illustrative of the technical solution of the present invention and unrestricted, although logical
Cross above preferred embodiment the present invention is described in detail, it is to be understood by those skilled in the art that can be
Various changes are made to it in form and in details, without departing from claims of the present invention limited range.
Claims (9)
1. the preparation method of canopy scattered seed, it is characterised in that comprise the following steps：
A, in mass ratio be 1-3：1-3：1-3：1-3：1-3：1-3：1-3：1-3 take respectively Chinese ephedra, fry semen armeniacae amarae, roasted perilla fruit,
Dried orange peel, honey-fried CORTEX MORI, Poria cocos and honey-fried licorice root, the water for then adding 6~12 times equivalent to medicinal material gross mass carry out first time decoction,
Filtrate is collected by filtration, the water that the dregs of a decoction add 4~10 times equivalent to medicinal material gross mass carries out second of decoction, filter is collected by filtration
Liquid, the water that the dregs of a decoction add 3-8 times equivalent to medicinal material gross mass carries out third time decoction, and filtrate is collected by filtration；
B, 3 decoction filtrates of merging, filtration, filter vacuum are concentrated under reduced pressure into the concentrate that relative density is 1.12~1.18；
C, using the mixture of dextrin and lactose as substrate, spray into concentrate obtained by step b, fluidized drying plasmid, screen grain
The particle in 16-60 mesh is spent, canopy scattered seed is obtained.
2. the preparation method of canopy scattered seed according to claim 1, it is characterised in that：The Chinese ephedra, stir-fry semen armeniacae amarae, stir-fry are purple
Perillaseed, dried orange peel, honey-fried CORTEX MORI, the mass ratio of Poria cocos and honey-fried licorice root are 3：3：3：3：3：3：1.5.
3. the preparation method of canopy scattered seed according to claim 1, it is characterised in that：The first time decocting time is 1
~3 hours, second of decocting time was 1~1.5 hour, and the third time decocting time is 0.5~1.5 hour.
4. the preparation method of canopy scattered seed according to claim 1, it is characterised in that：In step c, the dextrin and lactose
Mass ratio be 3:1.
5. the preparation method of canopy scattered seed according to claim 1, it is characterised in that：The fluidized drying condition is air intake
Temperature：80 DEG C, blower fan frequency 35Hz, charging rate 40rmin-1, atomizing pressure 0.1Mpa.
6. the preparation method of canopy scattered seed according to claim 1, it is characterised in that：The mixture of the dextrin and lactose
Addition is 1.12 times of dry cream amount.
7. the method for quality control of canopy scattered seed, it is characterised in that comprise the following steps：
(1) ephedrine hydrochloride, the measure of pseudoephedrine hydrochloride content：Canopy scattered seed is taken, methanol solution is added after grinding, ultrasound is molten
Solution, cooling, then add methanol solution to supply weightlessness, shake up, filter, collect filtrate and obtain canopy powder particulate samples；Ephedrine hydrochloride, salt
Sour pseudoephedrine standard items methanol solution dissolves, and shakes up to obtain standard solution, then by canopy powder particulate samples and standard items
Solution is detected under following chromatographic condition：Chromatographic column：Length and a diameter of 250mm × 4.6mm, 5 μm of Kromasil100-
5Phenyl；Column temperature：27℃；Sample size：10μl；Flow velocity：1.0ml·min-1；Mobile phase：Acetonitrile is with phosphoric acid quality fraction
0.1% phosphoric acid water volume ratio is 1: 99；Detection wavelength：210nm；
(2) measure of liquiritin, aurantiamarin, rosmarinic acid contents：Take and methanol solution is used after canopy powder particulate abrasive, canopy is made
Then liquiritin, aurantiamarin, Rosmarinic acid standard items are added methanol to dissolve by scattered seed sample, are made standard solution, then by China
Lid scattered seed sample and standard solution are detected under following chromatographic condition：Chromatographic column：Length and diameter 250 × 4.6mm, 5 μm
Thermo Syncronis C18；Column temperature：27℃；Mobile phase：The phosphoric acid water of acetonitrile -0.01%；Sample size：20μl；Flow velocity：
1.0ml·min-1；Mobile phase：Acetonitrile and the phosphoric acid water gradient elution that phosphoric acid quality fraction is 0.1%, 0~12min acetonitrile volumes
Than for 18%, 12~30min acetonitriles volume ratio is 20%, 30~40min acetonitriles volume ratio is 25%, 40~55min acetonitrile bodies
Product is than being 100%；
(3) result judges：Canopy powder particulate samples are in ephedrine hydrochloride, pseudoephedrine hydrochloride, liquiritin, aurantiamarin and rosemary
Appearance meets quality standard at sour standard items appearance.
8. the method for quality control of canopy scattered seed according to claim 7, it is characterised in that in step (1), canopy powder
Grain sample preparation methods be：Canopy scattered seed is taken, adds the hydrochloric volume fractions of 250ml by 3 every gram of canopy scattered seeds after grinding
For 50% methanol solution, ultrasonic dissolution, cooling, then the methanol solution for adding hydrochloric volume fraction to be 50% supply weightlessness,
Shake up, filter, collect filtrate and obtain canopy powder particulate samples；Hydrochloric acid mass fraction is 0.036% in the methanol solution；
Standard solution preparation method is：Ephedrine hydrochloride, pseudoephedrine hydrochloride are weighed respectively, with the first that volume fraction is 50%
Alcohol dissolves and diluted, and it is respectively 20 μ g/ml, 10 μ g/ml solution to be configured to hydrochloric ephedrine, pseudoephedrine hydrochloride.
9. the method for quality control of canopy scattered seed according to claim 7, it is characterised in that in step (2), canopy powder
Grain sample preparation methods be：Canopy scattered seed is taken, adds 100ml methanol by every gram of canopy scattered seed, in frequency 40kHz, power
Ultrasonic extraction 30min under the conditions of 240W, takes out, and cooling supplies weightlessness, in 10000rmin-110min is centrifuged, supernatant is used
0.45 μm of miillpore filter filtration；
Standard solution preparation method is：Liquiritin, aurantiamarin, Rosmarinic acid are weighed respectively, plus methanol dissolving is configured to concentration
Respectively 0.3733mgml-1、0.0902mg·ml-1And 0.1911mgml-1Solution.
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| CN109856270A (en) * | 2019-01-29 | 2019-06-07 | 浙江医药高等专科学校 | A method of with 7 index components in hplc simultaneous determination canopy powder granule |
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| CN109856270A (en) * | 2019-01-29 | 2019-06-07 | 浙江医药高等专科学校 | A method of with 7 index components in hplc simultaneous determination canopy powder granule |
| CN110346323A (en) * | 2019-07-30 | 2019-10-18 | 江西中医药大学 | A method of based on near-infrared spectrum technique on-line checking canopy powder concentrate |
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| CN112345675B (en) * | 2020-12-07 | 2022-08-05 | 葵花药业集团湖北武当有限公司 | HPLC method for simultaneously detecting 8 active ingredients in infantile Magan granules |
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Application publication date: 20170926 |