CN109613166A - A kind of head luxuriant growth Tongbian capsule quality determining method - Google Patents
A kind of head luxuriant growth Tongbian capsule quality determining method Download PDFInfo
- Publication number
- CN109613166A CN109613166A CN201910038114.8A CN201910038114A CN109613166A CN 109613166 A CN109613166 A CN 109613166A CN 201910038114 A CN201910038114 A CN 201910038114A CN 109613166 A CN109613166 A CN 109613166A
- Authority
- CN
- China
- Prior art keywords
- solution
- reference substance
- luxuriant growth
- tongbian capsule
- growth tongbian
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
Abstract
The invention belongs to analysising drug form of Chinese materia medica fields, specifically disclose a kind of first luxuriant growth Tongbian capsule quality determining method, the quality determining method identifies cassia seed, fructus lycii and Rhizoma Atractylodis Macrocephalae in first luxuriant growth Tongbian capsule with thin-layered chromatography, 2 in first luxuriant growth Tongbian capsule are measured with HPLC method, 3, the content of 5,4'- tetrahydroxystilbene -2-O- β-D-Glucose glycosides, aurantiin, neohesperidin and barbaloin.Quality determining method of the present invention is reliable and stable, specificity is strong, favorable reproducibility, can fully and effectively control the quality of first luxuriant growth Tongbian capsule, be conducive to stabilized product quality, it is ensured that clinical application safely, effectively, to preferably meet the needs in medical treatment and market.
Description
Technical field
The present invention relates to a kind of Chinese patent drug head luxuriant growth Tongbian capsule quality determining methods, belong to analysising drug form of Chinese materia medica field.
Background technique
First luxuriant growth Tongbian capsule is 6 kind new medicine of Chinese medicine that Lunan Pharmaceutical Co., Ltd. develops, and is exclusive product, in
Acquisition on May 6th, 2015 produces official written reply (national drug standard Z20150041) and New Drug Certificate (traditional Chinese medicines demonstrate,prove word Z20150005),
Success lists.
First luxuriant growth Tongbian capsule prescription derives from clinical experience side, by the fleece-flower root, aloe, cassia seed, fructus lycii, donkey-hide gelatin, people
Ginseng, Rhizoma Atractylodis Macrocephalae, dried immature fruit of citron orange eight traditional chinese medicines composition.This prescription with theory of traditional Chinese medical science be guidance, merge clinical experience, relax bowel and defecation, rush down it is turbid
It is aided with the product of nourishing blood for moistening dryness in the product of toxin expelling, helps with the product of air making-up and spleen enlivening, make to drop the flavour of a drug of the turbid ruffian that disappears, reasonable recipe, compatibility
Precise and appropriate, gas yin with mending, be not detained by tonification and purgation in combination, benefit, rushes down and does not hurt just, by supplementing qi and nourishing yin, improves constitution and reach treatment constipation
Purpose.We especially to accumulate in malicious heresy, constipation caused by yin-fluid virtual loss has good relax bowel and defecation therapeutic effect, can be comprehensive
Improve gastrointestinal function, curative for effect, rapid-action, no toxicity, and has effects that toxin-expelling and face nourishing, Weight-reducing and lipid-lowering.Clinic is answered
With showing that its is curative for effect, important function is played to treatment functional consitipation, has been suitble to the elderly and the patient having a delicate constitution clothes
With firmly getting doctors and patients' favorable comment.
Chinese patent CN106124685A discloses a kind of quality determining method of first luxuriant growth Tongbian capsule, including uses thin layer
Chromatography identifies ginseng, the dried immature fruit of citron orange, aloe and donkey-hide gelatin medicinal material in preparation respectively, in the HPLC measurement fleece-flower root 2,3,5,4'- tetra-
Naringin content in hydroxy diphenyl ethylene -2-O- β-D-Glucose glycosides content and the dried immature fruit of citron orange.
Summary of the invention
The technical problem to be solved by the present invention is in Chinese patent CN106124685A " the quality inspection of first luxuriant growth Tongbian capsule
On the basis of survey method ", the quality determining method of first luxuriant growth Tongbian capsule is advanced optimized, increases cassia seed, fructus lycii and white
The thin layer of three taste raw medicinal material of art identifies, in process of production can be to the aloe in product, cassia seed, fructus lycii, donkey-hide gelatin, people
7 kinds of ginseng, Rhizoma Atractylodis Macrocephalae, dried immature fruit of citron orange medicinal materials while Qualitive test, reach multicomponent and jointly control.Meanwhile in order to simplify operation, detection is improved
Efficiency, inventor is by exploration for a long time and test repeatedly, successfully by 2,3,5,4'- tetra- hydroxyls in first luxuriant growth Tongbian capsule
The HPLC assay conjunction of base talan -2-O- β-D-Glucose glycosides, 4 kinds of aurantiin, neohesperidin and/or barbaloin ingredients
And it is one, a kind of new method more comprehensively and accurately detecting first luxuriant growth defaecation quality is provided.
The object of the present invention is to provide a kind of first luxuriant growth Tongbian capsule quality determining method, the head luxuriant growth Tongbian capsule is by what
The tuber of multiflower knotweed, aloe, cassia seed, fructus lycii, donkey-hide gelatin, ginseng, Rhizoma Atractylodis Macrocephalae, dried immature fruit of citron orange eight traditional chinese medicines prescription, extracted, purifying are made.This hair
Bright head luxuriant growth Tongbian capsule quality determining method is to identify cassia seed, fructus lycii and/or Rhizoma Atractylodis Macrocephalae in preparation with thin-layered chromatography, with
HPLC measures 2,3,5,4'- tetrahydroxystilbene -2-O- β-D-Glucose glycosides, aurantiin, new orange in first luxuriant growth Tongbian capsule
The content of skin glycosides and barbaloin realizes thoroughly evaluating to first luxuriant growth Tongbian capsule quality and control, thus headed by luxuriant growth Tongbian capsule
The true and false identify and the detection of inherent quality superiority and inferiority provides accurate foundation.
Above-mentioned technical proposal of the present invention is with cassia seed, fructus lycii and Rhizoma Atractylodis Macrocephalae in indentification by TLC head luxuriant growth Tongbian capsule, tool
Body includes the following steps:
1. thin-layered chromatography identifies the cassia seed in first luxuriant growth Tongbian capsule:
1) prepared by test solution: taking first luxuriant growth Tongbian capsule content appropriate, adds methanol ultrasonic, filtration is evaporated, residue adds
Water dissolution, then plus hydrochloric acid, heating water bath is cooling, and extracted by ether, ether extracted liquid is evaporated, and residue adds methanol to dissolve, as examination
Product solution.
2) prepared by reference substance solution: taking aurantio-obtusin reference substance, adds methanol that solution of every 1mL containing 1mg is made, as right
According to product solution.
3) point sample, expansion: test solution, reference substance solution are drawn respectively, point is on same silica gel g thin-layer plate, with first
Benzene-acetic ether-methanoic acid is solvent, is unfolded, and takes out, dries, and develops the color, inspects.
Preferably, the thin-layered chromatography identify the cassia seed in first luxuriant growth Tongbian capsule the following steps are included:
1) prepared by test solution: taking first luxuriant growth Tongbian capsule content appropriate, adds methanol ultrasonic, filtration is evaporated, residue adds
Water dissolution, then plus hydrochloric acid, heating water bath is cooling, and with extracted by ether, ether extracted liquid is evaporated, and residue adds methanol to dissolve, as confession
Test sample solution.
2) prepared by reference substance solution: taking aurantio-obtusin reference substance, adds methanol that solution of every 1mL containing 1mg is made, as right
According to product solution.
3) point sample, expansion: test solution, reference substance solution are drawn respectively, point is on same silica gel g thin-layer plate, with first
Benzene-acetic ether-methanoic acid=10:1:0.3 be solvent, be unfolded, take out, dry, set smoked in ammonia steam it is clear to spot development；
In sample chromatogram, at the position corresponding to the chromatogram of the reference substance, the spot of same color is shown.
2. thin-layered chromatography identifies the fructus lycii in first luxuriant growth Tongbian capsule:
1) prepared by test solution: take first luxuriant growth Tongbian capsule content appropriate, ultrasound, and centrifugation, supernatant ethyl acetate
It extracts；Acetic acid ethyl acetate extract is taken, is extracted with ammonia solution；Ammonia solution extracting solution is taken, with dilute hydrochloric acid tune pH value, then uses ethyl acetate
It extracts, acetic acid ethyl acetate extract is evaporated, and residue adds ethyl acetate to dissolve, as test solution.
2) prepared by control medicinal material solution: taking fructus lycii control medicinal material, adds water, boil, let cool, filters, filtrate acetic acid second
Ester extracts, and divides and takes acetic acid ethyl acetate extract, is evaporated, residue adds ethyl acetate to dissolve, as control medicinal material solution.
3) point sample, expansion: drawing test solution, control medicinal material solution respectively, point on same silica gel g thin-layer plate, with
Chloroform-methanol is solvent, is unfolded, and takes out, dries, inspect.
Preferably, the thin-layered chromatography identify the fructus lycii in first luxuriant growth Tongbian capsule the following steps are included:
1) prepared by test solution: it takes first luxuriant growth Tongbian capsule content appropriate, adds water ultrasonic, centrifugation, and supernatant acetic acid
Ethyl ester extracts, and point takes acetic acid ethyl acetate extract, is extracted with ammonia solution, point takes ammonia solution extracting solution, with dilute hydrochloric acid tune pH value to 3,
It is extracted with ethyl acetate again, acetic acid ethyl acetate extract is evaporated, and residue adds ethyl acetate to dissolve, as test solution；
2) prepared by control medicinal material solution: taking fructus lycii control medicinal material 0.5g, adds water, heating is boiled 15 minutes, let cool, and is filtered
It crosses, filtrate is extracted with ethyl acetate, and divides and takes acetic acid ethyl fluid, is evaporated, residue adds ethyl acetate to dissolve, molten as control medicinal material
Liquid；
3) point sample, expansion: drawing test solution, control medicinal material solution respectively, point on same silica gel g thin-layer plate, with
Chloroform: methanol=15:1 is solvent, is unfolded, and takes out, dries, set ultraviolet lamp and inspect under 365nm；Sample chromatogram
In, on position corresponding with reference medicine chromatography, show the fluorescence spot of same color.
3. thin-layered chromatography identifies the Rhizoma Atractylodis Macrocephalae in first luxuriant growth Tongbian capsule:
1) prepared by test solution: it takes first luxuriant growth Tongbian capsule content appropriate, adds water ultrasonic, centrifugation, and supernatant ether
It extracts, ether extracted liquid is evaporated, and residue adds methanol to dissolve, as test solution.
2) prepared by control medicinal material solution: taking Rhizoma Atractylodis Macrocephalae control medicinal material, adds water, heating and refluxing extraction filters, and filtrate concentration is put
Cold, extracted by ether, ether extracted liquid is evaporated, and residue adds methanol to dissolve, as control medicinal material solution.
3) point sample, expansion: drawing test solution, control medicinal material solution respectively, point on same silica gel g thin-layer plate, with
Cyclohexane-ethyl acetate-formic acid is solvent, is unfolded, and takes out, dries, and develops the color, inspects.
Preferably, the thin-layered chromatography identify the Rhizoma Atractylodis Macrocephalae in first luxuriant growth Tongbian capsule the following steps are included:
1) prepared by test solution: it takes first luxuriant growth Tongbian capsule content appropriate, adds water ultrasonic, centrifugation, and supernatant ether
It extracts, ether extracted liquid is evaporated, and residue adds methanol to dissolve, as test solution；
2) prepared by control medicinal material solution: taking Rhizoma Atractylodis Macrocephalae control medicinal material 0.5g, adds water, heating and refluxing extraction filters, and filtrate is dense
Contracting, lets cool, extracted by ether, ether extracted liquid is evaporated, and residue adds methanol to dissolve, as control medicinal material solution；
3) point sample, expansion: test solution, reference substance solution are drawn respectively, point is on same silica gel g thin-layer plate, with ring
Hexane: ethyl acetate: formic acid=5:5:0.2 is solvent, is unfolded, and takes out, dries, and sprays with 2% sodium hydroxide solution, sets ultraviolet
Light lamp is inspected under 365nm；In sample chromatogram, on position corresponding with reference medicine chromatography, the fluorescence of same color is shown
Spot.
The present invention is also with 2,3,5,4'- tetrahydroxy hexichol of the fleece-flower root in high effective liquid chromatography for measuring head luxuriant growth Tongbian capsule
Ethylene -2-O- β-D-Glucose glycosides, the aurantiin of the dried immature fruit of citron orange and neohesperidin, aloe barbaloin content, specifically include following step
It is rapid:
1) prepared by test solution: taking first luxuriant growth Tongbian capsule content appropriate, sets in measuring bottle, methanol is added to dissolve, constant volume surpasses
Sound is let cool, and is shaken up, filtration, as test solution；
2) prepared by reference substance solution: precision weighs 2,3,5,4'- tetrahydroxystilbene -2-O- β-D-Glucose glycosides control
Product, aurantiin reference substance, neohesperidin reference substance and barbaloin reference substance are appropriate, set in volumetric flask, and methanol is added to dissolve and dilute
To scale, shake up to obtain the final product；
3) HPLC chromatogram condition: gradient elution is carried out by mobile phase of -0.1% phosphoric acid solution of acetonitrile；Detection wavelength
283nm-355nm；
4) measuring method: it is accurate respectively to draw reference substance solution and test solution, liquid chromatograph is injected, according to step
3) chromatographic condition measurement to get.
Preferably, 2,3,5,4'- tetrahydroxy hexichol in the high effective liquid chromatography for measuring head luxuriant growth Tongbian capsule preparation
Ethylene -2-O- β-D-Glucose glycosides, aurantiin, neohesperidin and barbaloin content the following steps are included:
1) prepared by test solution: take first luxuriant growth Tongbian capsule content appropriate, it is finely ground, and about 0.25g is taken, it is accurately weighed, it sets
In 100mL measuring bottle, adds 50% methanol to scale, be ultrasonically treated 30 minutes, let cool, shake up, filter, as test solution；
2) prepared by reference substance solution: precision weighs 2,3,5,4'- tetrahydroxystilbene -2-O- β-D-Glucose glycosides control
Product, aurantiin reference substance, neohesperidin reference substance and barbaloin reference substance are appropriate, set in volumetric flask, and methanol is added to dissolve and dilute
To scale, shake up to obtain the final product；
3) HPLC chromatogram condition: gradient elution is carried out by mobile phase of -0.1% phosphoric acid solution of acetonitrile；Detection wavelength
283nm-355nm；4) measuring method: it is accurate respectively to draw reference substance solution and 5 μ L of test solution, liquid chromatograph is injected,
According to chromatographic condition described in step 3) measure to get.
Preferably, high performance liquid chromatography step 3) gradient elution program are as follows:
| 0 | Acetonitrile (%) | 0.1% phosphoric acid solution (%) |
| 0-40 | 12% → 23% | 88% → 77% |
| 40-60 | 23% → 23% | 77% → 77%. |
Preferably, high performance liquid chromatography step 3) wavelength changeover program are as follows:
Wavelength switching: 0-26min, 320nm detect 2,3,5,4'- tetrahydroxystilbene -2-O- β-D-Glucose glycosides；
26min-39min, 283nm detect aurantiin and neohesperidin；39min-60min, 355nm detect barbaloin.
The present invention establishes first luxuriant growth Tongbian capsule upgrade version quality determining method, and this method is right respectively using thin-layered chromatography
Cassia seed, fructus lycii and Rhizoma Atractylodis Macrocephalae carry out Qualitive test in first luxuriant growth Tongbian capsule, reach multicomponent and jointly control；HPLC is used simultaneously
Quantitative determine 2,3,5,4'- tetrahydroxystilbene -2-O- β-D-Glucose glycosides, aurantiin, the new orange in first luxuriant growth Tongbian capsule
The content of skin glycosides and barbaloin further can effectively control the quality of first luxuriant growth Tongbian capsule, realize and carry out entirely to the quality of the pharmaceutical preparations
Evaluate to face.
It is operated to simplify, improves the detection efficiency of HPLC method assay, inventor by exploring and instead for a long time
Multiple test, by the long switching method of gradient elution program parallel connection multiplex successfully by 2,3,5,4'- tetra- in first luxuriant growth Tongbian capsule
The HPLC assay conjunction of hydroxy diphenyl ethylene -2-O- β-D-Glucose glycosides, 4 kinds of aurantiin, neohesperidin and barbaloin ingredients
And it is one, provide a kind of new method for more comprehensively, accurately, easily detecting first luxuriant growth defaecation quality.Quality testing of the present invention
Method is reliable and stable, specificity is strong, favorable reproducibility, can fully and effectively control the quality of first luxuriant growth Tongbian capsule, be conducive to stablize
The quality of product, it is ensured that clinical application safety and validity preferably meet the needs in medical treatment and market.
Detailed description of the invention
Headed by Fig. 1 in luxuriant growth Tongbian capsule cassia seed thin-layer chromatogram, by sequence from left to right, wherein 1 is to lack Cassia
The negative formulation samples of son, 2,4 be aurantio-obtusin reference substance, and 3 be sample；
Headed by Fig. 2 in luxuriant growth Tongbian capsule fructus lycii thin-layer chromatogram, by sequence from left to right, wherein 1,4 be fructus lycii
Sub- control medicinal material, 2 be the negative formulation samples for lacking fructus lycii, and 3 be sample；
Headed by Fig. 3 in luxuriant growth Tongbian capsule Rhizoma Atractylodis Macrocephalae thin-layer chromatogram, by sequence from left to right, wherein 1,4 be Rhizoma Atractylodis Macrocephalae pair
According to medicinal material, 2 be the negative formulation samples for lacking Rhizoma Atractylodis Macrocephalae, and 3 be sample；
Fig. 4 is reference substance HPLC chromatogram, and chromatographic peak is from left to right followed successively by 2,3,5,4'- tetrahydroxystilbene -2-
O- β-D-Glucose glycosides, aurantiin, neohesperidin, barbaloin；
Fig. 5 is test sample HPLC chromatogram；
Fig. 6 is to lack fleece-flower root negative control HPLC chromatogram；
Fig. 7 is to lack dried immature fruit of citron orange negative control HPLC chromatogram；
Fig. 8 is to lack aloe negative control HPLC chromatogram.
Specific embodiment
12,3,5,4'- tetrahydroxystilbene -2-O- β of embodiment-D-Glucose glycosides, aurantiin, neohesperidin and reed
The HPLC mensuration methodology of luxuriant growth glycosides is studied
1) drug and reagent: 2,3,5,4'- tetrahydroxystilbene -2-O- β-D-Glucose glycosides reference substance (110844-
2000607, Nat'l Pharmaceutical & Biological Products Control Institute), aurantiin reference substance (110722-201312, Chinese pharmaceutical biological product inspection
Determine institute), neohesperidin reference substance (111857-201703, Nat'l Pharmaceutical & Biological Products Control Institute), barbaloin reference substance
(110787-201808, Nat'l Pharmaceutical & Biological Products Control Institute), acetonitrile, methanol are chromatographically pure, remaining reagent is that analysis is pure,
Water is double distilled water.
2) instrument: 1100 high performance liquid chromatograph of AgiLent, DAD detector.
3) chromatographic condition: chromatographic column: KromasiL C18 chromatographic column (4.6mm × 250mm, 5 μm)；Mobile phase: acetonitrile
(A) -0.1% phosphoric acid solution (B) gradient elution, gradient elution program are shown in Table 1；Detection wavelength: 283nm-355nm, wavelength switching
Program is shown in Table 2；Flow velocity: 1mL/min.
1 gradient elution program of table
| Time (min) | Mobile phase A (%) | Mobile phase B (%) |
| 0-40 | 12% → 23% | 88% → 77% |
| 40-60 | 23% → 23% | 77% → 77% |
2 wavelength changeover program of table
| Time (min) | Detection wavelength (nm) |
| 0-26 | 320 |
| 26-39 | 283 |
| 39-60 | 355。 |
4) prepared by solution
4.1) preparation of test solution
Take first luxuriant growth Tongbian capsule content appropriate, it is finely ground, about 0.25g is taken, it is accurately weighed, it sets in 100mL measuring bottle, adds 50%
Methanol is ultrasonically treated 30 minutes to scale, lets cool, shake up, filter, as test solution.
4.2) preparation of reference substance solution
Precision weighs 2,3,5,4'- tetrahydroxystilbene -2-O- β-D-Glucose glycosides reference substance, aurantiin, new orange peel
Glycosides, barbaloin reference substance are appropriate, add methanol that every 1mL is made containing 0.4988mg, 0.5006mg, 0.71225mg, 0.72072mg
Mixed solution to get.
4.3) preparation of negative control solution
The negative control without polygonum multiflorum medicinal material, the negative control without Fructus Aurantii Immaturus, not aloetic feminine gender are taken respectively
Control operates with method according under the preparation of test solution, negative control solution is made, from chromatogram as can be seen that 2,3,
It is noiseless at 5,4'- tetrahydroxystilbene -2-O- β-D-Glucose glycosides, aurantiin, neohesperidin and barbaloin position, see figure
4, Fig. 5, Fig. 6, Fig. 7, Fig. 8.
5) linear relationship is investigated
It is appropriate that precision weighs each reference substance, adds methanol to be made into following concentration, is measured under above-mentioned chromatographic condition, respectively
5 μ L of sample introduction measures peak area.It the results are shown in Table 3,4,5,6.
32,3,5,4'- tetrahydroxystilbene -2-O- β of table-D-Glucose glycosides linear relationship investigates result
4 aurantiin linear relationship of table investigates result
5 neohesperidin linear relationship of table investigates result
6 barbaloin linear relationship of table investigates result
2,3,5,4'- tetrahydroxystilbene -2-O- β-D-Glucose glycosides measurement, it is right to measure peak area as ordinate
It is abscissa according to product concentration (mg/mL), draws standard curve, obtain regression equation Y=36684131.91660X-23900.5, r=
0.99986, i.e., 2,3,5,4'- tetrahydroxystilbene -2-O- β-D-Glucose glycosides concentration is in 0.009976~0.04988mg/
It is linear good within the scope of mL.
Aurantiin measurement, to measure peak area as ordinate, reference substance concentration (mg/mL) is abscissa, and it is bent to draw standard
Line, obtains regression equation Y=19359268.87735X-13015.0, r=0.99979, i.e., aurantiin concentration 0.020024~
It is linear good within the scope of 0.10012mg/mL.
Neohesperidin measurement, to measure peak area as ordinate, reference substance concentration (mg/mL) is abscissa, draws standard
Curve, obtains regression equation Y=20767730.61313X-14830.12, r=0.99992, i.e. neohesperidin concentration exists
It is linear good within the scope of 0.014245~0.071225mg/mL.
Barbaloin measurement, to measure peak area as ordinate, reference substance concentration (mg/mL) is abscissa, and it is bent to draw standard
Line, obtains regression equation Y=14884500.22200X+26595.10, r=0.99971, i.e., barbaloin concentration 0.072072~
It is linear good within the scope of 0.360360mg/mL.
6) precision test
Precision draws reference substance solution under 4.2) item, repeats sample introduction 6 times, 5 μ L, peak area RSD < 2% show instrument every time
Precision is good.It the results are shown in Table 7.
7 Precision test result of table
7) stability test
Same test solution under 4.1) item is taken, 0,2,4,6, the 8h measurement after preparation, the results showed that test sample is molten
Liquid is stablized in 8h.It the results are shown in Table 8.
8 stability test result of table
8) repetitive test
6 parts of sample of same lot number (07015001) are taken respectively, are operated according to the sample solution preparation method under 4.1) item,
It measures respectively, calculates content.It the results are shown in Table 9,10,11,12.
92,3,5,4'- tetrahydroxystilbene -2-O- β of table-D-Glucose glycosides repetitive test result
10 aurantiin repetitive test result of table
11 neohesperidin repetitive test result of table
12 barbaloin repetitive test result of table
9) recovery test
Precision weighs 6 parts of sample of known content, respectively accurate 2,3,5, the 4'- tetrahydroxys two that 0.4988mg/ml is added
Styrene -2-O- β-D-Glucose glycosides reference substance solution 2mL, 0.5006mg/ml aurantiin reference substance solution 5ml,
The barbaloin reference substance solution 5ml of neohesperidin reference substance solution 2ml, 1.7mg/ml of 0.71225mg/ml, under 4.1) item
Sample solution preparation method preparation, measurement.It the results are shown in Table 13,14,15,16.
13 2,3,5,4'- tetrahydroxystilbene -2-O- β of table-D-Glucose glycosides recovery test result
14 aurantiin recovery test result of table
15 neohesperidin recovery test result of table
16 barbaloin recovery test result of table
Embodiment 2-4
1) drug and reagent: with embodiment 1；
2) instrument: with embodiment 1；
3) chromatographic condition: with embodiment 1；
4) prepared by solution
4.1) preparation of test solution
Take 07015001,07015002,07015003 batch head luxuriant growth Tongbian capsule content appropriate respectively, it is finely ground, it takes about
0.25g, it is accurately weighed, it sets in 100mL measuring bottle, adds 50% methanol to scale, ultrasonic treatment 30 minutes lets cool, shakes up, it filters,
As test solution.
4.2) preparation of reference substance solution
With embodiment 1
5) it measures:
Above-mentioned each batch head luxuriant growth Tongbian capsule test solution, reference substance solution are taken, high performance liquid chromatograph is injected separately into,
It is measured according to the chromatographic condition under 3) item, records chromatogram.
6) result: separating degree is high between each ingredient, and noiseless between each other, each component content is as shown in table 17.
2,3,5,4'- tetrahydroxystilbene -2-O- β-D-Glucose glycosides in 17 different batches head luxuriant growth Tongbian capsule of table,
The content of aurantiin, neohesperidin, barbaloin
Cassia seed indentification by TLC in the first luxuriant growth Tongbian capsule of embodiment 5
1) preparation of test solution: taking 07015001 batch head luxuriant growth Tongbian capsule content 6g, finely ground, adds methanol
30ml, ultrasonic extraction 30 minutes, filtration, be evaporated, residue adds water 20ml to make to dissolve, then plus hydrochloric acid 2ml, set heating water bath 30 and divide
Clock cools down immediately, with extracted by ether 2 times, each 20ml, merges ether solution, is evaporated, residue adds methanol 1ml to make to dissolve, as confession
Test sample solution.
2) preparation of reference substance solution: taking aurantio-obtusin reference substance, adds methanol that solution of every 1mL containing 1mg is made, as
Reference substance solution.
3) point sample, expansion: each 2 μ L of above two solution is drawn, is put respectively on same silica gel g thin-layer plate, with toluene-second
Acetoacetic ester-formic acid=10:1:0.3 be solvent, be unfolded, take out, dry, set smoked in ammonia steam it is clear to spot development.
4) result: headed by Fig. 1 in luxuriant growth Tongbian capsule cassia seed thin-layer chromatogram, the results showed that the sample containing cassia seed
Product show the spot of same color on position corresponding with aurantio-obtusin reference substance chromatography.Chromatographic isolation is good, cassia seed
Characteristic spots are prominent, and the TLC method of foundation can be used as the quality determining method of cassia seed in first luxuriant growth Tongbian capsule.
Fructus lycii indentification by TLC in the first luxuriant growth Tongbian capsule of embodiment 6
1) preparation of test solution: taking 07015002 batch head luxuriant growth Tongbian capsule content 4g, finely ground, adds water 30mL,
Ultrasound 30 minutes, centrifugation, supernatant are extracted 1 time with ethyl acetate 30ml, are divided and are taken ethyl acetate layer, are extracted with ammonia solution 10ml,
Divide and take ammonium hydroxide layer, with dilute hydrochloric acid tune pH value to 3, is extracted with ethyl acetate 20ml, acetic acid ethyl fluid is evaporated, and residue adds ethyl acetate
1mL makes to dissolve, as test solution.
2) preparation of control medicinal material solution: taking fructus lycii control medicinal material 0.5g, adds water 35ml, and heating is boiled 15 minutes, put
Cold, filtration, filtrate is extracted with ethyl acetate 15ml, is divided and is taken acetic acid ethyl fluid, is evaporated, and residue adds ethyl acetate 1ml to make to dissolve, and is made
For control medicinal material solution.
3) point sample, expansion: test solution, each 5 μ L of control medicinal material solution are drawn, is put respectively in same silica gel g thin-layer plate
On, using chloroform: methanol=15:1 is unfolded as solvent, takes out, dries, set ultraviolet lamp and inspect under 365nm.
4) result: headed by Fig. 2 in luxuriant growth Tongbian capsule fructus lycii thin-layer chromatogram, the results showed that the sample containing fructus lycii
Product show the fluorescence spot of same color on position corresponding with fructus lycii reference medicine chromatography.Chromatographic isolation is good, fructus lycii
Characteristic spots it is prominent, the TLC method of foundation can be used as the quality determining method of fructus lycii in first luxuriant growth Tongbian capsule.
Rhizoma Atractylodis Macrocephalae indentification by TLC in the first luxuriant growth Tongbian capsule of embodiment 7
1) preparation of test solution: taking 07015003 batch head luxuriant growth Tongbian capsule content 4g, finely ground, adds water 30mL,
Ultrasonic treatment 30 minutes, centrifugation, supernatant are merged ether extracted liquid, are volatilized, residue adds first with extracted by ether 2 times, each 20ml
Alcohol 1ml makes to dissolve, as test solution.
2) preparation of control medicinal material solution: taking Rhizoma Atractylodis Macrocephalae control medicinal material 0.5g, add water 50ml, is heated to reflux 30 minutes, filtration,
Filtrate is concentrated into about 30ml, lets cool, and with extracted by ether 2 times, each 20ml, merges ether extracted liquid, is evaporated, residue adds methanol
1ml makes to dissolve, as control medicinal material solution.
3) point sample, expansion: drawing each 5 μ L of above two solution, put respectively on same silica gel g thin-layer plate, with hexamethylene:
Ethyl acetate: formic acid=5:5:0.2 is solvent, is unfolded, and takes out, dries, and sprays with 2% sodium hydroxide solution, sets ultraviolet lamp
It is inspected under 365nm.
4) result: headed by Fig. 3 in luxuriant growth Tongbian capsule Rhizoma Atractylodis Macrocephalae thin-layer chromatogram, the results showed that the sample containing Rhizoma Atractylodis Macrocephalae exists
On position corresponding with Rhizoma Atractylodis Macrocephalae reference medicine chromatography, the fluorescence spot of same color is shown.Chromatographic isolation is good, the feature spot of Rhizoma Atractylodis Macrocephalae
Point protrusion, the TLC method of foundation can be used as the quality determining method of Rhizoma Atractylodis Macrocephalae in first luxuriant growth Tongbian capsule.
Therefore above embodiments are only the preferred embodiment of the present invention, and the description thereof is more specific and detailed, but can not be
And it is interpreted as limitations on the scope of the patent of the present invention.It should be pointed out that for those of ordinary skill in the art, not departing from
Under the premise of the principle of the invention and design, several modifications and improvement can also be made, these are all within the scope of protection of the present invention.
Claims (10)
1. a kind of head luxuriant growth Tongbian capsule quality determining method, which is characterized in that this method identifies first luxuriant growth defaecation with thin-layered chromatography
Cassia seed, fructus lycii and/or Rhizoma Atractylodis Macrocephalae in capsule, in high effective liquid chromatography for measuring head luxuriant growth Tongbian capsule 2,3,5,4'- tetra-
The content of hydroxy diphenyl ethylene -2-O- β-D-Glucose glycosides, aurantiin, neohesperidin and/or barbaloin.
2. quality determining method as described in claim 1, which is characterized in that the thin-layered chromatography identifies first luxuriant growth Tongbian capsule
In cassia seed the following steps are included:
1) prepared by test solution: taking first luxuriant growth Tongbian capsule content appropriate, adds methanol ultrasonic, filtration is evaporated, residue adds water-soluble
Solution, then plus hydrochloric acid, heating water bath is cooling, and extracted by ether, ether extracted liquid is evaporated, and residue adds methanol to dissolve, molten as test sample
Liquid；
2) prepared by reference substance solution: taking aurantio-obtusin reference substance, adds methanol that solution of every 1mL containing 1mg is made, as reference substance
Solution；
3) point sample, expansion: test solution, reference substance solution are drawn respectively, point is on same silica gel g thin-layer plate, with toluene-second
Acetoacetic ester-formic acid is solvent, is unfolded, and takes out, dries, and develops the color, inspects.
3. quality determining method as claimed in claim 2, which is characterized in that with toluene-ethyl acetate-first in the step 3)
Acid=10:1:0.3 is solvent.
4. quality determining method as described in claim 1, which is characterized in that the thin-layered chromatography identifies first luxuriant growth Tongbian capsule
In fructus lycii the following steps are included:
1) prepared by test solution: taking first luxuriant growth Tongbian capsule content appropriate, ultrasound is centrifuged, and supernatant is extracted with ethyl acetate；
Acetic acid ethyl acetate extract is taken, is extracted with ammonia solution；Ammonia solution extracting solution is taken, with dilute hydrochloric acid tune pH value, then is extracted with ethyl acetate,
Acetic acid ethyl acetate extract is evaporated, and residue adds ethyl acetate to dissolve, as test solution；
2) prepared by control medicinal material solution: taking fructus lycii control medicinal material, adds water, boil, let cool, filter, filtrate is mentioned with ethyl acetate
It takes, divides and take acetic acid ethyl acetate extract, be evaporated, residue adds ethyl acetate to dissolve, as control medicinal material solution；
3) point sample, expansion: test solution, control medicinal material solution are drawn respectively, point is on same silica gel g thin-layer plate, with trichlorine
Methane-methanol is solvent, is unfolded, and takes out, dries, inspect.
5. quality determining method as claimed in claim 4, which is characterized in that with chloroform in the step 3): methanol=
15:1 is solvent.
6. quality determining method as described in claim 1, which is characterized in that the thin-layered chromatography identifies first luxuriant growth Tongbian capsule
In Rhizoma Atractylodis Macrocephalae the following steps are included:
1) prepared by test solution: it takes first luxuriant growth Tongbian capsule content appropriate, adds water ultrasonic, centrifugation, and supernatant extracted by ether,
Ether extracted liquid is evaporated, and residue adds methanol to dissolve, as test solution；
2) prepared by control medicinal material solution: taking Rhizoma Atractylodis Macrocephalae control medicinal material, adds water, heating and refluxing extraction filters, and filtrate concentration is let cool, second
Ether extracts, and ether extracted liquid is evaporated, and residue adds methanol to dissolve, as control medicinal material solution；
3) point sample, expansion: test solution, control medicinal material solution are drawn respectively, point is on same silica gel g thin-layer plate, with hexamethylene
Alkane-acetic ether-methanoic acid is solvent, is unfolded, and takes out, dries, and develops the color, inspects.
7. quality determining method as claimed in claim 6, which is characterized in that with hexamethylene in the step 3): ethyl acetate:
Formic acid=5:5:0.2 is solvent.
8. quality determining method as described in claim 1, which is characterized in that the high effective liquid chromatography for measuring head luxuriant growth defaecation
2 in capsule preparations, 3,5,4'- tetrahydroxystilbene -2-O- β-D-Glucose glycosides, aurantiin, neohesperidin and barbaloin
Content, comprising the following steps:
1) prepared by test solution: taking first luxuriant growth Tongbian capsule content appropriate, sets in volumetric flask, methanol is added to dissolve, constant volume surpasses
Sound is let cool, and is shaken up, filtration, as test solution；
2) reference substance solution prepare: precision weigh 2,3,5,4'- tetrahydroxystilbene -2-O- β-D-Glucose glycosides reference substance,
Aurantiin reference substance, neohesperidin reference substance and barbaloin reference substance are appropriate, set in volumetric flask, add methanol to dissolve and are diluted to quarter
Degree, shakes up to obtain the final product；
3) HPLC chromatogram condition: gradient elution is carried out by mobile phase of -0.1% phosphoric acid solution of acetonitrile；Detection wavelength 283nm-
355nm；
4) measuring method: it is accurate respectively to draw reference substance solution and test solution, liquid chromatograph is injected, according to step 3) institute
State chromatographic condition measurement to get；
Preferably, 2,3,5, the 4'- tetrahydroxystilbenes-in the high effective liquid chromatography for measuring head luxuriant growth Tongbian capsule preparation
2-O- β-D-Glucose glycosides, aurantiin, neohesperidin and barbaloin content the following steps are included:
1) prepared by test solution: take first luxuriant growth Tongbian capsule content appropriate, it is finely ground, and about 0.25g is taken, it is accurately weighed, set 100mL
In measuring bottle, adds 50% methanol to scale, be ultrasonically treated 30 minutes, let cool, shake up, filter, as test solution；
2) reference substance solution prepare: precision weigh 2,3,5,4'- tetrahydroxystilbene -2-O- β-D-Glucose glycosides reference substance,
Aurantiin reference substance, neohesperidin reference substance and barbaloin reference substance are appropriate, set in volumetric flask, add methanol to dissolve and are diluted to quarter
Degree, shakes up to obtain the final product；
3) HPLC chromatogram condition: gradient elution is carried out by mobile phase of -0.1% phosphoric acid solution of acetonitrile；Detection wavelength 283nm-
355nm；
4) measuring method: it is accurate respectively to draw reference substance solution and 5 μ L of test solution, liquid chromatograph is injected, according to step
3) chromatographic condition measurement to get.
9. according to the method described in claim 8, it is characterized in that, the high performance liquid chromatography step 3) gradient elution program
Are as follows:
10. method according to claim 8 or claim 9, which is characterized in that high performance liquid chromatography step 3) the wavelength switching
Program are as follows:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910038114.8A CN109613166B (en) | 2019-01-16 | 2019-01-16 | Quality detection method of 'Jihui Tongbiang' capsule |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910038114.8A CN109613166B (en) | 2019-01-16 | 2019-01-16 | Quality detection method of 'Jihui Tongbiang' capsule |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109613166A true CN109613166A (en) | 2019-04-12 |
| CN109613166B CN109613166B (en) | 2020-01-07 |
Family
ID=66019648
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910038114.8A Active CN109613166B (en) | 2019-01-16 | 2019-01-16 | Quality detection method of 'Jihui Tongbiang' capsule |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109613166B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111272943A (en) * | 2020-03-24 | 2020-06-12 | 广西中医药大学第一附属医院 | Quality detection method of spleen-tonifying and qi-benefiting oral liquid |
| CN111624295A (en) * | 2020-07-02 | 2020-09-04 | 鲁南厚普制药有限公司 | Quality detection method of 'Jihui Tongbiang' capsule |
| CN112067725A (en) * | 2020-09-19 | 2020-12-11 | 湖南时代阳光药业股份有限公司 | Construction method of standard fingerprint of yitong tablets and method for determining component content of yitong tablets |
| CN113332373A (en) * | 2021-07-14 | 2021-09-03 | 鲁南制药集团股份有限公司 | Application of aloe cathartic preparation in preparing medicine for treating vomiting |
| CN113406241A (en) * | 2021-07-14 | 2021-09-17 | 鲁南制药集团股份有限公司 | Quality detection method of Xintong granules |
Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1876139A (en) * | 2005-06-03 | 2006-12-13 | 贵阳云岩西创药物科技开发有限公司 | Medicinal preparation for treating children's fastidium, its preparation process and quality control method |
| CN1887324A (en) * | 2005-06-27 | 2007-01-03 | 仁和（集团）发展有限公司 | Chinese composition and its prepn process and quality control method |
| CN101224233A (en) * | 2007-01-19 | 2008-07-23 | 重庆生态药物研究所 | Cassia plant extract and extracting method thereof |
| CN101336986A (en) * | 2007-07-06 | 2009-01-07 | 王�锋 | Medicine composition and preparation method and quality control method thereof |
| CN101417038A (en) * | 2007-10-23 | 2009-04-29 | 北京亚东生物制药有限公司 | Traditional Chinese medicine composition for treating male infertility, preparation method and quality control method thereof |
| CN101518619A (en) * | 2009-04-02 | 2009-09-02 | 吉林省辉南长龙生化药业股份有限公司 | Compound brain activation and comfort capsule and quality control method thereof |
| CN102038921A (en) * | 2009-10-26 | 2011-05-04 | 天津中新药业集团股份有限公司达仁堂制药厂 | Quality control method of meridian warming pill as traditional Chinese medical preparation |
| CN102998410A (en) * | 2011-09-13 | 2013-03-27 | 天士力制药集团股份有限公司 | Blood nourishing and brain arousing particle quality detection method |
| CN104306500A (en) * | 2014-10-17 | 2015-01-28 | 叶祖光 | Method for detecting medicine for treating irritable bowel syndrome |
| CN106123496A (en) * | 2016-06-30 | 2016-11-16 | 鲁南制药集团股份有限公司 | A kind of drying means of Chinese medical concrete |
| CN106124685A (en) * | 2016-06-10 | 2016-11-16 | 鲁南厚普制药有限公司 | The quality determining method of first luxuriant growth Tongbian capsule |
| CN107966516A (en) * | 2018-01-10 | 2018-04-27 | 广西壮族自治区食品药品检验所 | A kind of discrimination method of Xiao Ke Lin piece and Xiaokelin capsule for diabetes |
| CN108956846A (en) * | 2018-07-27 | 2018-12-07 | 河北中医学院 | A kind of shipi powder freeze-dried powder multiple medicine taste multi information, quick thin-layer identification method |
-
2019
- 2019-01-16 CN CN201910038114.8A patent/CN109613166B/en active Active
Patent Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1876139A (en) * | 2005-06-03 | 2006-12-13 | 贵阳云岩西创药物科技开发有限公司 | Medicinal preparation for treating children's fastidium, its preparation process and quality control method |
| CN1887324A (en) * | 2005-06-27 | 2007-01-03 | 仁和（集团）发展有限公司 | Chinese composition and its prepn process and quality control method |
| CN101224233A (en) * | 2007-01-19 | 2008-07-23 | 重庆生态药物研究所 | Cassia plant extract and extracting method thereof |
| CN101336986A (en) * | 2007-07-06 | 2009-01-07 | 王�锋 | Medicine composition and preparation method and quality control method thereof |
| CN101417038A (en) * | 2007-10-23 | 2009-04-29 | 北京亚东生物制药有限公司 | Traditional Chinese medicine composition for treating male infertility, preparation method and quality control method thereof |
| CN101518619A (en) * | 2009-04-02 | 2009-09-02 | 吉林省辉南长龙生化药业股份有限公司 | Compound brain activation and comfort capsule and quality control method thereof |
| CN102038921A (en) * | 2009-10-26 | 2011-05-04 | 天津中新药业集团股份有限公司达仁堂制药厂 | Quality control method of meridian warming pill as traditional Chinese medical preparation |
| CN102998410A (en) * | 2011-09-13 | 2013-03-27 | 天士力制药集团股份有限公司 | Blood nourishing and brain arousing particle quality detection method |
| CN104306500A (en) * | 2014-10-17 | 2015-01-28 | 叶祖光 | Method for detecting medicine for treating irritable bowel syndrome |
| CN106124685A (en) * | 2016-06-10 | 2016-11-16 | 鲁南厚普制药有限公司 | The quality determining method of first luxuriant growth Tongbian capsule |
| CN106123496A (en) * | 2016-06-30 | 2016-11-16 | 鲁南制药集团股份有限公司 | A kind of drying means of Chinese medical concrete |
| CN107966516A (en) * | 2018-01-10 | 2018-04-27 | 广西壮族自治区食品药品检验所 | A kind of discrimination method of Xiao Ke Lin piece and Xiaokelin capsule for diabetes |
| CN108956846A (en) * | 2018-07-27 | 2018-12-07 | 河北中医学院 | A kind of shipi powder freeze-dried powder multiple medicine taste multi information, quick thin-layer identification method |
Non-Patent Citations (6)
| Title |
|---|
| 孟楣 等: "薄层色谱法鉴别枸杞子的实验研究", 《中国药事》 * |
| 张丹丹 等: "3种中药成方制剂中何首乌、虎杖、决明子薄层鉴别方法的建立", 《中南药学》 * |
| 戚雁飞 等: "幼泻宁颗粒质量标准研究", 《浙江中医药大学学报》 * |
| 李玉基 等: "甜梦合剂的质量标准研究", 《食品与药品》 * |
| 陈丹 等: "HPLC法测定便秘舒胶囊中芦荟苷含量", 《中草药》 * |
| 高效液相色谱法测定便通胶囊中柚皮苷和新橙皮苷的含量: "汪勇良 等", 《中国生化药物杂志》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111272943A (en) * | 2020-03-24 | 2020-06-12 | 广西中医药大学第一附属医院 | Quality detection method of spleen-tonifying and qi-benefiting oral liquid |
| CN111272943B (en) * | 2020-03-24 | 2023-12-05 | 广西中医药大学第一附属医院 | Quality detection method of spleen-strengthening and qi-tonifying oral liquid |
| CN111624295A (en) * | 2020-07-02 | 2020-09-04 | 鲁南厚普制药有限公司 | Quality detection method of 'Jihui Tongbiang' capsule |
| CN111624295B (en) * | 2020-07-02 | 2022-11-08 | 鲁南厚普制药有限公司 | Quality detection method of 'Jihui Tongbiang' capsule |
| CN112067725A (en) * | 2020-09-19 | 2020-12-11 | 湖南时代阳光药业股份有限公司 | Construction method of standard fingerprint of yitong tablets and method for determining component content of yitong tablets |
| CN112067725B (en) * | 2020-09-19 | 2022-04-08 | 湖南时代阳光药业股份有限公司 | Standard fingerprint spectrum construction method of Yitong tablet and method for measuring its component content |
| CN113332373A (en) * | 2021-07-14 | 2021-09-03 | 鲁南制药集团股份有限公司 | Application of aloe cathartic preparation in preparing medicine for treating vomiting |
| CN113406241A (en) * | 2021-07-14 | 2021-09-17 | 鲁南制药集团股份有限公司 | Quality detection method of Xintong granules |
| CN113406241B (en) * | 2021-07-14 | 2022-09-13 | 鲁南制药集团股份有限公司 | Detection method of Xintong granules |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109613166B (en) | 2020-01-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109613166A (en) | A kind of head luxuriant growth Tongbian capsule quality determining method | |
| CN106124685B (en) | Quality detection method of fallopia multiflora (thunb.) harald-aloe constipation relieving capsules | |
| CN105467059B (en) | A kind of quality determining method for the Chinese medicine composition for treating blood urine | |
| CN102590433B (en) | A kind of quality determining method of the smooth preparation of liver | |
| CN106370749A (en) | Quality detection method of ginseng basis-consolidating oral solution | |
| CN102323371B (en) | Detection method of haemostasis medicine | |
| CN106198837A (en) | The quality determining method of old cough with asthma sheet | |
| CN108760945A (en) | A kind of detection method of Qijiaoshenbai capsule | |
| CN102218122B (en) | Detection method for sea dragon and gecko oral liquid | |
| CN106324117B (en) | The quality determining method of Longbi Xintong granule | |
| CN103344737A (en) | Quality control method of traditional Chinese medicine tablet for treating nasosinusitis | |
| CN109239220B (en) | A kind of quality determining method of Yupingfeng Granules | |
| CN101204434A (en) | Quality standard for thrombus dispelling pill and test method thereof | |
| CN102228645A (en) | Quality control method for traditional Chinese medicine composition for treating infantile indigestion with food retention | |
| CN102068549B (en) | Detection method for Chinese medicinal preparation heat clearing and blood cooling pills | |
| CN106153812A (en) | A kind of detection method of the Chinese medicine preparation treating endometriosis | |
| CN109406682A (en) | The UPLC characteristic spectrum construction method and detection method of ginger medicinal material | |
| CN102068627A (en) | Quality control method for Chinese medicine preparation Xinnaojing tabelets | |
| CN106442843A (en) | Quality check method of children's granules for clearing heat from throat | |
| CN105300997B (en) | A kind of detection method of the pharmaceutical preparation treating gynecological inflammation | |
| CN102091297A (en) | Quality control method for liver health care medicine | |
| CN105004833B (en) | It is a kind of treat acute gouty arthritis, gout Chinese medicine preparation detection method | |
| CN105628853B (en) | A kind of quality determining method of cymbopogon distans medicinal material | |
| CN106706766B (en) | A kind of measuring method of the newly-increased detection ingredient of Chinese medicine Tang blade that treating AIDS | |
| CN100570358C (en) | Treat the detection method of asthenopic pharmaceutical preparation |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Zhang Guimin Inventor after: Li Yinkun Inventor after: Zhuang Huifang Inventor after: Deng Lihua Inventor before: Li Yinkun Inventor before: Zhuang Huifang Inventor before: Deng Lihua |