CN106093262A - A kind of method of the finger printing of the pharmaceutical preparation setting up Radix Scrophulariae - Google Patents
A kind of method of the finger printing of the pharmaceutical preparation setting up Radix Scrophulariae Download PDFInfo
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- CN106093262A CN106093262A CN201610423663.3A CN201610423663A CN106093262A CN 106093262 A CN106093262 A CN 106093262A CN 201610423663 A CN201610423663 A CN 201610423663A CN 106093262 A CN106093262 A CN 106093262A
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- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
Abstract
The method that the present invention relates to the finger printing of a kind of pharmaceutical preparation setting up Radix Scrophulariae.The method, with Radix Scrophulariae granule for detection object, the method establishing the finger printing for this pharmaceutical preparation, obtain more comprehensively profile information, confirm S peak, common characteristic peak harpagoside, No. 1 peak Harpagide, No. 2 peaks and No. 3 peak cinnamic acid, select S peak harpagoside, determine the relative retention time at the common characteristic peak of Radix Scrophulariae granule, and combine the information of multiple chromatographic peaks in this finger printing, can be all sidedly, detect its quality rapidly, be conducive to the detection of its total quality and global quality control, thus it is favorably improved the safety and stability of this drug use.Meanwhile, the method has the advantages such as stability is high, precision is high, reproducible.
Description
Technical field
The invention belongs to pharmaceutical analysis field, be specifically related to the side of the finger printing of a kind of pharmaceutical preparation setting up Radix Scrophulariae
Method.
Background technology
Radix Scrophulariae granule is by Studying Chinese Crude Drug Figwort root extracts, concentrates, pelletizes gained.Radix Scrophulariae is goatweed
The dry root of Scrophularia ningpoensis Hemsl., begins to be loaded in Shennong's Herbal, and Radix Scrophulariae is distributed mainly on east
North, North China and East China；There is effect of removing heat from blood YIN nourishing, eliminating fire and detoxication, be mainly used in consumption of YIN caused by febrile disease, crimson tongue excessive thirst, temperature poison
Send out speckle, Tianjin and hinder the treatment of constipation, hectic fever due to YIN-deficiency chronic cough, conjunctival congestion, pharyngalgia, scrofula, diphtheria, carbuncle sore tumefacting virus etc..The Radix Scrophulariae mainly ether Han cyclenes
Terpene glycoside, Phenylpropanoid Glycosides glycoside, fragrance glucosides class etc., wherein cyclenes fan terpene glycoside mainly refers to containing Harpagide and harpagoside isoreactivity
Mark composition.
" Chinese Pharmacopoeia " version in 2015 includes former plant variety, Medicinal Materials Characters, physicochemical identification, contains the quality control of Radix Scrophulariae
Measuring the projects such as fixed, chemical composition in Radix Scrophulariae is also illustrated by document, including containing the cyclenes fan such as Harpagide and harpagoside
Terpene glycoside and the composition such as Phenylpropanoid Glycosides glycoside, fragrance glucosides class, but effective ingredient type such for Radix Scrophulariae granule is many, group
Point complicated Chinese medicine preparation, only measures the content of certain constituents, it is difficult to objective, effectively evaluate or control the quality of medical material.
But, on the one hand, by assay or the discriminating Radix Scrophulariae granule of above-mentioned single component, it is impossible on the whole
Detect and control its quality；On the other hand, the discriminating Radix Scrophulariae formula of other compositions is combined by the assay of single component
Grain, time-consuming, laborious, it is difficult to be widely used in production practices.
Therefore, set up a kind of method that can detect Radix Scrophulariae granule all sidedly, rapidly, its total quality is examined
Survey and global quality control is significant.
Summary of the invention
It is that the single Testing index of detection method of existing Radix Scrophulariae granule can not be to this end, to be solved by this invention
Detect and control its quality, multiple Testing index joint-detection on the whole time-consuming, laborious, it is difficult to be widely used in production practices
Technical problem, thus the method proposing the finger printing of a kind of pharmaceutical preparation setting up Radix Scrophulariae.
For solving above-mentioned technical problem, the present invention is achieved through the following technical solutions:
The present invention provides the method for the finger printing of a kind of pharmaceutical preparation setting up Radix Scrophulariae, and the method comprises the steps:
(1) the pharmaceutical preparation 0.4-0.6 weight portion of Radix Scrophulariae to be measured is taken, accurately weighed, accurate addition 40～60% methanol-water
Solution 40-60 parts by volume, weighed weight, heating and refluxing extraction or supersound extraction 20-40 minute, let cool, more weighed weight, take 40
～60% methanol aqueous solution supply the weight of less loss, shake up, filter, take subsequent filtrate, as need testing solution；
(2) precision weighs Harpagide reference substance, adds 40～60% methanol aqueous solution makes every 1 parts by volume containing 0.00004-
The solution of 0.00008 weight portion, shakes up, as reference substance solution A；
Precision weighs harpagoside reference substance, adds 40～60% methanol aqueous solution makes every 1 parts by volume containing 0.00001-
The solution of 0.00003 weight portion, shakes up, as reference substance B solution；
Precision weighs cinnamic acid reference substance, adds 40～60% methanol aqueous solution makes every 1 parts by volume containing 0.00001-
The solution of 0.00003 weight portion, shakes up, as reference substance C solution；
(3) chromatographic condition: with octadecylsilane chemically bonded silica as filler, with acetonitrile as mobile phase A, with 0.05%
Phosphoric acid solution is that Mobile phase B carries out gradient elution according to following program: 0-10min, A:B are 5%:95% → 8%:92%；10-
20min, A:B are 8%:92% → 22%:78%；20-25min, A:B are 22%:78% → 27.5%:72.5%；25-
30min, A:B are 27.5%:72.5% → 28%:72%；30-40min, A:B are 28%:72% → 35%:65%；40-
45min, A:B are 35%:65% → 100%:0%；Detection wavelength is 210nm (0～18min) and 278nm (18～45min)；
Column temperature is 25 DEG C, and flow velocity is 1mL/min；
(4) respectively precision draw need testing solution need testing solution, reference substance solution A and, reference substance B solution and reference substance
C solution 0.010-0.020 parts by volume, injects high performance liquid chromatograph, measures, and obtains need testing solution, reference substance solution A respectively
With, reference substance B solution and the liquid chromatograph of reference substance C solution；
(5) Chinese Pharmacopoeia Commission's similarity evaluation is utilized, to need testing solution, comparison
Product solution A and, the liquid chromatograph of reference substance B solution and reference substance C solution import respectively through data, Supplements and data
Join, obtain finger printing；
Described weight portion is g/mL with the relation of described parts by volume.
Preferably, the method for the finger printing of the above-mentioned pharmaceutical preparation setting up Radix Scrophulariae of the present invention, the method includes walking as follows
Rapid:
(1) pharmaceutical preparation 0.5 weight portion of Radix Scrophulariae to be measured is taken, accurately weighed, accurate addition 50% methanol aqueous solution 50 body
Long-pending part, weighed weight, heating and refluxing extraction or supersound extraction 30 minutes, let cool, more weighed weight, takes 50% methanol aqueous solution and mends
The weight of foot less loss, shakes up, and filters, takes subsequent filtrate, as need testing solution；
(2) precision weighs Harpagide reference substance, adds 50% methanol aqueous solution and makes every 1 parts by volume containing 0.00006 weight portion
Solution, shake up, as reference substance solution A；
Precision weighs harpagoside reference substance, adds 50% methanol aqueous solution and makes every 1 parts by volume containing 0.00002 weight portion
Solution, shakes up, as reference substance B solution；
Precision weighs cinnamic acid reference substance, adds 40～60% methanol aqueous solution makes every 1 parts by volume containing 0.00002 weight portion
Solution, shake up, as reference substance C solution；
(3) chromatographic condition: with octadecylsilane chemically bonded silica as filler, with acetonitrile as mobile phase A, with 0.05%
Phosphoric acid solution is that Mobile phase B carries out gradient elution according to following program: 0-10min, A:B are 5%:95% → 8%:92%；10-
20min, A:B are 8%:92% → 22%:78%；20-25min, A:B are 22%:78% → 27.5%:72.5%；25-
30min, A:B are 27.5%:72.5% → 28%:72%；30-40min, A:B are 28%:72% → 35%:65%；40-
45min, A:B are 35%:65% → 100%:0%；Detection wavelength is 210nm (0～18min) and 278nm (18～45min)；
Column temperature is 25 DEG C, and flow velocity is 1mL/min；
(4) respectively precision draw need testing solution need testing solution, reference substance solution A and, reference substance B solution and reference substance
C solution 0.015 parts by volume, inject high performance liquid chromatograph, measure, respectively need testing solution, reference substance solution A and, comparison
Product B solution and the liquid chromatograph of reference substance C solution；
(5) Chinese Pharmacopoeia Commission's similarity evaluation is utilized, to need testing solution, comparison
Product solution A and, the liquid chromatograph of reference substance B solution and reference substance C solution import respectively through data, Supplements and data
Join, obtain finger printing.
It is further preferred that the method for the finger printing of the above-mentioned pharmaceutical preparation setting up Radix Scrophulariae of the present invention, with 4.6mm ×
250mm, Agilent Zorbax SB-C18,4.6mm × 250mm of 5 μm, 5 μm Diamonsil C18 or 4.6mm ×
250mm, the Shim-pack VP-ODS of 5 μm are chromatographic column.
It is further preferred that the method for the finger printing of the above-mentioned pharmaceutical preparation setting up Radix Scrophulariae of the present invention, described medicine system
Agent is tablet, capsule, pill, granule, honey refining pill, slow releasing preparation, quick releasing formulation, controlled release preparation, oral liquid
Or ejection preparation.
It is further preferred that the method for the finger printing of the above-mentioned pharmaceutical preparation setting up Radix Scrophulariae of the present invention, described Radix Scrophulariae
Pharmaceutical preparation is prepared by the following method and forms:
Take Radix Scrophulariae, heating and refluxing extraction at least 1 time, add the water extraction at least 0.5h of at least 2 weight times amount, mistake every time
Filter, merging filtrate, it is 1.10～1.15 that filtrate is concentrated into 60 DEG C of relative densities, adds customary adjuvant, according to common process, makes
The most acceptable tablet, capsule, pill, granule, honey refining pill, slow releasing preparation, quick releasing formulation, controlled release preparation, mouth
Take liquid preparation or ejection preparation.
It is further preferred that the method for the finger printing of the above-mentioned pharmaceutical preparation setting up Radix Scrophulariae of the present invention, described Radix Scrophulariae
Pharmaceutical preparation is prepared by the following method and forms:
Take Radix Scrophulariae, heating and refluxing extraction 1～5 times, add the water extraction 0.5～3.0h of 4～10 weight times amount, mistake every time
Filter, merging filtrate, it is 1.10～1.15 that filtrate is concentrated into 60 DEG C of relative densities, adds customary adjuvant, according to common process, makes
The most acceptable tablet, capsule, pill, granule, honey refining pill, slow releasing preparation, quick releasing formulation, controlled release preparation, mouth
Take liquid preparation or ejection preparation.
It is further preferred that the method for the finger printing of the above-mentioned pharmaceutical preparation setting up Radix Scrophulariae of the present invention, described Radix Scrophulariae
Pharmaceutical preparation is prepared by the following method and forms:
Take Radix Scrophulariae, heating and refluxing extraction 2 times, the water extraction 2.0h that the 1st time adds 8 weight times amount, add 6 weight the 2nd time
The water extraction 1.5h of times amount, filters, merging filtrate, and it is 1.10～1.15 that filtrate is concentrated into 60 DEG C of relative densities, adds conventional auxiliary
Material, according to common process, make the most acceptable tablet, capsule, pill, granule, honey refining pill, slow releasing preparation,
Quick releasing formulation, controlled release preparation, oral liquid or ejection preparation.
Described pharmaceutically acceptable adjuvant is: filler, disintegrating agent, lubricant, suspending agent, binding agent, sweeting agent, rectify
Taste agent, preservative, substrate etc..Filler includes: starch, pregelatinized Starch, lactose, mannitol, chitin, microcrystalline Cellulose,
Sucrose etc.；Disintegrating agent includes: starch, pregelatinized Starch, microcrystalline Cellulose, carboxymethyl starch sodium, crospolyvinylpyrrolidone,
Low-substituted hydroxypropyl cellulose, cross-linked carboxymethyl cellulose are received；Lubricant includes: magnesium stearate, sodium lauryl sulphate, Talcum
Powder, silicon dioxide etc.；Suspending agent includes: polyvinylpyrrolidone, microcrystalline Cellulose, sucrose, agar, hydroxypropyl methyl cellulose
Deng；Binding agent includes, starch slurry, polyvinylpyrrolidone, hydroxypropyl methyl cellulose etc.；Sweeting agent includes: saccharin sodium, A Si
Pa Tan, sucrose, cyclamate, enoxolone etc.；Correctives includes: sweeting agent and various essence；Preservative includes: parabens,
Benzoic acid, sodium benzoate, sorbic acid and its esters, benzalkonium bromide, fixed, the eucalyptus oil of acetic acid chloroethene etc.；Substrate includes: PEG6000,
PEG4000, insect wax etc..
It is further preferred that the method for the finger printing of the above-mentioned pharmaceutical preparation setting up Radix Scrophulariae of the present invention, described Radix Scrophulariae
In the finger printing of pharmaceutical preparation, common characteristic peak is: S peak harpagoside, No. 1 peak Harpagide, No. 2 peaks and No. 3 peak cinnamic acid,
With S peak harpagoside for internal reference peak, each peak relative retention time be respectively as follows: No. 1 peak 0.22～0.26, No. 2 peaks 0.75～
0.89, S peak 1.00 and No. 3 peaks 1.06～1.24.
It is further preferred that the method for the finger printing of the above-mentioned pharmaceutical preparation setting up Radix Scrophulariae of the present invention, described Radix Scrophulariae
In the finger printing of pharmaceutical preparation, each peak relative retention time is respectively as follows: peak 0.82, No. 1 peak 0.24,2, S peak 1.00 and 3
Number peak 1.15.
The present invention also provides for said method application in the quality testing and quality control of the pharmaceutical preparation of Radix Scrophulariae.
Compared with prior art, the technique scheme of the present invention has the advantage that
The detection method of the finger printing of the pharmaceutical preparation of Radix Scrophulariae of the present invention is right with Radix Scrophulariae granule for detection
As, the method establishing the finger printing for this pharmaceutical preparation, it is thus achieved that more comprehensively profile information, it is thus identified that total spy
Levy S peak, peak harpagoside, No. 1 peak Harpagide, No. 2 peaks and No. 3 peak cinnamic acid, select S peak harpagoside, it is determined that Radix Scrophulariae formula
The relative retention time at the common characteristic peak of granule, and combine the information of multiple chromatographic peaks in this finger printing, it is possible to all sidedly,
Detect its quality rapidly, be conducive to the detection of its total quality and global quality control, thus be favorably improved this drug use
Safety and stability.Meanwhile, the method has the advantages such as stability is high, precision is high, reproducible.
Accompanying drawing explanation
In order to make present disclosure be more likely to be clearly understood, below according to the specific embodiment of the present invention and combine
Accompanying drawing, the present invention is further detailed explanation, wherein:
Fig. 1 is the chromatogram of detection wavelength different in experimental example 1 of the present invention, and peak 1 is Harpagide, and S peak is harpagoside,
The detection wavelength of chromatogram 1,2 is 210nm+280nm, and the detection wavelength of chromatogram 3,4 is 210nm+278nm；
Fig. 2 is the chromatogram of different flowing phases, A: acetonitrile-0.03% phosphoric acid solution in experimental example 1 of the present invention；B: acetonitrile-
0.04% phosphoric acid solution；C: acetonitrile-0.05% phosphoric acid solution；D: acetonitrile-0.06% phosphoric acid solution；
Fig. 3 is the chromatogram of different gradient elution program, A: gradient 1 in experimental example 1 of the present invention；B: gradient 2；C: gradient 3；
Fig. 4 is the chromatogram of different chromatographic columns in experimental example 1 of the present invention, I: Agilent Zorbax SB-C18 5 μm,
4.6mm×250mm PN:880975-902；II: Diamonsil (diamond) C18 (2) 5 μm 4.6mm × 250mm Ser#
201042495；III: Shim-pack VP-ODS 5 μm 4.6mm × 250mm S/N 07111129484；
Fig. 5 is the chromatogram of different in flow rate, A:0.8mL/min in experimental example 1 of the present invention；B:1.0mL/min；C:1.2mL/
min；
Fig. 6 is the chromatogram of different column temperatures in experimental example 1 of the present invention, A:25 DEG C；B:30 DEG C；C:35 DEG C；
Fig. 7 is the characteristic fingerprint pattern of 18 batches of Radix Scrophulariae granules in experimental example 3 of the present invention；
Fig. 8 is the comparison characteristic fingerprint pattern of Radix Scrophulariae granule in experimental example 3 of the present invention；
Fig. 9 is repeated experiment result in experimental example 4 of the present invention；
Figure 10 is Precision Experiment result in experimental example 4 of the present invention；
Figure 11 is specificity experimental result in experimental example 4 of the present invention, A: test sample；B: negative controls；
Figure 12 is stability of solution experimental result in experimental example 4 of the present invention.
Detailed description of the invention
Embodiment 1
In following example and experimental example, the preparation method of Radix Scrophulariae granule is: take Radix Scrophulariae, heating and refluxing extraction 2 times,
The water extraction 2.0h that 1st time adds 8 weight times amount, the water extraction 1.5h that the 2nd time adds 6 weight times amount, filter, merging filtrate,
It is 1.10～1.15 that filtrate is concentrated into 60 DEG C of relative densities, adds customary adjuvant, according to common process, makes granule.
Embodiment 2
The present embodiment sets up the method for the finger printing of Radix Scrophulariae granule, comprises the steps:
(1) the pharmaceutical preparation 0.5g of Radix Scrophulariae to be measured is taken, accurately weighed, the accurate 50% methanol aqueous solution 50mL that adds, weighed
Weight, supersound extraction 30 minutes, let cool, more weighed weight, take 50% methanol aqueous solution and supply the weight of less loss, shake up, filter,
Take subsequent filtrate, as need testing solution；
(2) precision weighs Harpagide reference substance, adds 50% methanol aqueous solution and makes every 1mL solution containing 0.00006g, shakes
Even, as reference substance solution A；
Precision weighs harpagoside reference substance, adds 50% methanol aqueous solution and makes every 1mL solution containing 0.00002g, shakes
Even, as reference substance B solution；
Precision weighs cinnamic acid reference substance, adds 40～60% methanol aqueous solution makes every 1 parts by volume containing 0.00002 weight portion
Solution, shake up, as reference substance C solution；
(3) chromatographic condition: with octadecylsilane chemically bonded silica as filler, with 4.6mm × 250mm, 5 μm
Agilent Zorbax SB-C18 is chromatographic column, the phosphoric acid solution with acetonitrile as mobile phase A, with 0.05% for Mobile phase B according to
Following program carries out gradient elution: 0-10min, A:B are 5%:95% → 8%:92%；10-20min, A:B be 8%:92% →
22%:78%；20-25min, A:B are 22%:78% → 27.5%:72.5%；25-30min, A:B are 27.5%:72.5%
→ 28%:72%；30-40min, A:B are 28%:72% → 35%:65%；40-45min, A:B be 35%:65% →
100%:0%；Detection wavelength is 210nm (0～18min) and 278nm (18～45min)；Column temperature is 25 DEG C, and flow velocity is 1mL/
min；
(4) respectively precision draw need testing solution, reference substance solution A and, reference substance B solution and reference substance C solution 0.015
Parts by volume, injects high performance liquid chromatograph, measures, respectively need testing solution, reference substance solution A and, reference substance B solution and right
Liquid chromatograph according to product C solution；
(5) Chinese Pharmacopoeia Commission's similarity evaluation is utilized, to need testing solution, comparison
Product solution A and, the liquid chromatograph of reference substance B solution and reference substance C solution import respectively through data, Supplements and data
Join, obtain finger printing.
Embodiment 3
The present embodiment sets up the method for the finger printing of Radix Scrophulariae granule, comprises the steps:
(1) the pharmaceutical preparation 0.4g of Radix Scrophulariae to be measured is taken, accurately weighed, the accurate 40% methanol aqueous solution 60mL that adds, weighed
Weight, supersound extraction 20 minutes, let cool, more weighed weight, take 40% methanol aqueous solution and supply the weight of less loss, shake up, filter,
Take subsequent filtrate, as need testing solution；
(2) precision weighs Harpagide reference substance, adds 40% methanol aqueous solution and makes every 1mL solution containing 0.00004g, shakes
Even, as reference substance solution A；
Precision weighs harpagoside reference substance, adds 40% methanol aqueous solution and makes every 1mL solution containing 0.00001g, shakes
Even, as reference substance B solution；
Precision weighs cinnamic acid reference substance, adds 40～60% methanol aqueous solution makes every 1 parts by volume containing 0.00001 weight portion
Solution, shake up, as reference substance C solution；
(3) chromatographic condition: with octadecylsilane chemically bonded silica as filler, with 4.6mm × 250mm, 5 μm
Agilent Zorbax SB-C18 is chromatographic column, the phosphoric acid solution with acetonitrile as mobile phase A, with 0.05% for Mobile phase B according to
Following program carries out gradient elution: 0-10min, A:B are 5%:95% → 8%:92%；10-20min, A:B be 8%:92% →
22%:78%；20-25min, A:B are 22%:78% → 27.5%:72.5%；25-30min, A:B are 27.5%:72.5%
→ 28%:72%；30-40min, A:B are 28%:72% → 35%:65%；40-45min, A:B be 35%:65% →
100%:0%；Detection wavelength is 210nm (0～18min) and 278nm (18～45min)；Column temperature is 25 DEG C, and flow velocity is 1mL/
min；
(4) respectively precision draw need testing solution, reference substance solution A and, reference substance B solution and reference substance C solution
0.010mL, inject high performance liquid chromatograph, measure, respectively need testing solution, reference substance solution A and, reference substance B solution and
The liquid chromatograph of reference substance C solution；
(5) Chinese Pharmacopoeia Commission's similarity evaluation is utilized, to need testing solution, comparison
Product solution A and, the liquid chromatograph of reference substance B solution and reference substance C solution import respectively through data, Supplements and data
Join, obtain finger printing.
Embodiment 4
The present embodiment sets up the method for the finger printing of Radix Scrophulariae granule, comprises the steps:
(1) the pharmaceutical preparation 0.6g of Radix Scrophulariae to be measured is taken, accurately weighed, the accurate 60% methanol aqueous solution 40mL that adds, weighed
Weight, supersound extraction 40 minutes, let cool, more weighed weight, take 60% methanol aqueous solution and supply the weight of less loss, shake up, filter,
Take subsequent filtrate, as need testing solution；
(2) precision weighs Harpagide reference substance, adds 60% methanol aqueous solution and makes every 1mL solution containing 0.00008g, shakes
Even, as reference substance solution A；
Precision weighs harpagoside reference substance, adds 60% methanol aqueous solution and makes every 1mL solution containing 0.00003g, shakes
Even, as reference substance B solution；
Precision weighs cinnamic acid reference substance, adds 40～60% methanol aqueous solution makes every 1 parts by volume containing 0.00003 weight portion
Solution, shake up, as reference substance C solution；
(3) chromatographic condition: with octadecylsilane chemically bonded silica as filler, with 4.6mm × 250mm, 5 μm
Agilent Zorbax SB-C18 is chromatographic column, the phosphoric acid solution with acetonitrile as mobile phase A, with 0.05% for Mobile phase B according to
Following program carries out gradient elution: 0-10min, A:B are 5%:95% → 8%:92%；10-20min, A:B be 8%:92% →
22%:78%；20-25min, A:B are 22%:78% → 27.5%:72.5%；25-30min, A:B are 27.5%:72.5%
→ 28%:72%；30-40min, A:B are 28%:72% → 35%:65%；40-45min, A:B be 35%:65% →
100%:0%；Detection wavelength is 210nm (0～18min) and 278nm (18～45min)；Column temperature is 25 DEG C, and flow velocity is 1mL/
min；
(4) respectively precision draw need testing solution, reference substance solution A and, reference substance B solution and reference substance C solution
0.020mL, inject high performance liquid chromatograph, measure, respectively need testing solution, reference substance solution A and, reference substance B solution and
The liquid chromatograph of reference substance C solution；
(5) Chinese Pharmacopoeia Commission's similarity evaluation is utilized, to need testing solution, comparison
Product solution A and, the liquid chromatograph of reference substance B solution and reference substance C solution import respectively through data, Supplements and data
Join, obtain finger printing.
Experimental example
1, instrument and reagent
Instrument includes: UltiMate 3000 chromatographic system, automatically enters including LPG-3400A quaternary pump, WPS-3000TSL
Sample device, PDA diode array detector, chromatographic work station；
Chromatographic column: Agilent Zorbax SB-C18 5 μm 4.6mm × 250mm PN:880975-902；Balance: 100,000
/ mono-balance (METTLER TOLEDO (Switzerland's prunus mume (sieb.) sieb.et zucc. Teller) XS-205), 100,000/balance (METTLER TOLEDO
(Switzerland's prunus mume (sieb.) sieb.et zucc. Teller) XP-56)；Supersonic generator: (SK5200H Shanghai High Kudos Science Instrument Co., Ltd.)；Ultrapure water system:
U.S. Millipore (Mi Libo) company.
Reagent and reagent include: acetonitrile is chromatographically pure (Sai Mo flies scientific and technological (Chinese) company limited of generation that), and water is ultra-pure water
(resistivity 18.2m Ω .cm), other reagent are analytical pure；Radix Scrophulariae granule (sequence number 1-18) is by China Resources three nine-day periods after the winter solstice medicine stock
Part company limited provides, and is prepared from according to the preparation method of embodiment 1.
Experimental example 1The determination of chromatographiccondition
(1) selection of wavelength is detected
Dual wavelength (210+278nm) and dual wavelength (210+280nm) is selected Radix Scrophulariae granule to be detected, no respectively
The chromatogram of same detection wavelength is as it is shown in figure 1, its retention time is as shown in table 1.
The retention time at each peak under table 1 different detection wavelength
From table 1 and Fig. 1, reporting in conjunction with document, peak 3 is cinnamic acid chromatographic peak, therefore Radix Scrophulariae granule characteristic spectrum
Detection wavelength selects dual wavelength (210+278nm).
(2) selection of the phase that flows
Investigation acetonitrile-0.03% phosphoric acid solution, acetonitrile-0.04% phosphoric acid solution, acetonitrile-0.05% phosphoric acid solution, acetonitrile-
The different flow phase system such as 0.06% phosphoric acid solution, the chromatogram of different flowing phases is as shown in Figure 2.As shown in Figure 2, acetonitrile-
0.05% phosphoric acid solution is preferable to each composition separating effect of Radix Scrophulariae granule, thus flow phase system determine employing acetonitrile-
0.05% phosphoric acid solution.
(3) selection of gradient
Granule ingredient is complicated, and isocratic elution is difficult to separate, therefore uses gradient elution mode.In experimentation
Have employed multiple different gradient to be measured, by relatively different eluting with a Radix Scrophulariae granule extraction sample
The sample chromatogram figure that program is measured, therefrom preferred color of choice spectrum information is abundanter, and main chromatographic peak separating degree is high, baseline relatively steadily and
The gradient that analysis time is relatively reasonable, different gradient elution program as shown in table 2～4, the chromatograph of different gradient elution program
Figure is as shown in Figure 3.
Table 2 gradient 1 (A: acetonitrile；B:0.05% phosphoric acid solution) elution program
Table 3 gradient 2 (A: acetonitrile；B:0.05% phosphoric acid solution) elution program
Table 4 gradient 3 (A: acetonitrile；B:0.05% phosphoric acid solution) elution program
From table 2～4 and Fig. 3, gradient 3 ratio gradient 1,2 good separating effect, the chromatogram peak shape that gradient 3 obtains is good,
Separating degree is high, and analysis time is more suitable, therefore determines that gradient 3 is final eluent gradient.
(4) investigation of different chromatographic columns
Take the need testing solution with a Radix Scrophulariae granule sample, respectively with chromatographic column I: Agilent Zorbax SB-
C18 5 μm 4.6mm × 250mm lot number: 880975-902；II: Diamonsil (diamond) C18 (2) 5 μm 4.6mm × 250mm
Lot number: Ser#201042495；III: Shim-pack VP-ODS5 μm 4.6mm × 250mm lot number: S/N 07111129484,
Carrying out gradient elution analysis by the flow velocity of 1.0mL/min, the chromatogram of different chromatographic columns is as shown in Figure 4, the most homochromy
The relative retention time result at the total peak that spectrum post measures is as shown in table 5.
The total chromatographic peak system suitability parameter that the different chromatographic column of table 5 measures
Preferable to the separating degree at each peak from Fig. 4 and Biao 5, Agilent Zorbax SB-C18 chromatographic column, and analyze
Time is shorter, therefore selected chromatographic column I is as chromatographic column.
(5) investigation of different in flow rate
Take the need testing solution with a Radix Scrophulariae granule sample, respectively with 0.8mL/min, 1.0mL/min, 1.2mL/
The different in flow rate such as min measures, and the chromatogram of different in flow rate is as it is shown in figure 5, different in flow rate when relatively retaining of total peak of measuring
Between result as shown in table 6.
The total chromatographic peak system suitability parameter that table 6 different in flow rate measures
From Fig. 5 and Biao 6, during flow velocity generation minor variations, the measurement result impact at each total peak is little, from system
Can be seen that in adaptability parameter, flow velocity is that the chromatograph effect of 1.0mL/min flow velocity is preferable.
(6) selection of different column temperatures
Take the need testing solution with a Radix Scrophulariae granule sample, investigate different column temperature 25 DEG C, 30 DEG C, 35 DEG C to this product
Separating effect, as shown in Figure 6, the relative retention time result at the total peak that different column temperatures measure is such as the chromatogram of different column temperatures
Shown in table 7.
The system suitability parameter at the total peak that the different column temperature of table 7 measures
From Fig. 6 and Biao 7, when column temperature changes, each chromatographic peak separating effect is close, shows that column temperature changes right
Measurement result impact is less.Mensuration environment can be made more stable in view of fixing column temperature, therefore the selected column temperature 25 close to room temperature
DEG C as the mensuration temperature of this method.
(7) final chromatographic condition
With octadecylsilane chemically bonded silica as filler；With acetonitrile as mobile phase A, 0.05% phosphoric acid solution is flowing phase
B, carries out gradient elution by table 8；Flow velocity 1.0mL/min, column temperature 25 DEG C；Detection wavelength: front 18min is 210nm, is changed to afterwards
278nm.Theoretical cam curve is calculated by harpagoside should be not less than 5000.
Table 8 gradient elution program
Experimental example 2The preparation of need testing solution
Precision weighs Radix Scrophulariae granule (lot number 1306001S) 5 groups, often organizes parallel 2 parts, and every part of 0.5g, precision adds respectively
Enter the water of 50mL, 30% methanol, 50% methanol, 70% methanol, 100% methanol, supersound extraction 30min.Less loss is supplied after letting cool
Solvent to original weight amount, shake up, filter, take subsequent filtrate with 0.45 μm filtering with microporous membrane, filtrate is as need testing solution.Respectively
Draw each test liquid 10 μ L, inject chromatograph of liquid, measure the integrating peak areas value of Harpagide and harpagoside.Radix Scrophulariae formula
Under grain various extracting conditions, Harpagide is as shown in table 9 with harpagoside integrating peak areas value.
Harpagide and harpagoside integrating peak areas value under table 9 Radix Scrophulariae granule various extracting conditions
As shown in Table 9, with H2O, 30%MeOH, 50%MeOH, 70%MeOH are Extraction solvent, Harpagide, harpagoside
Peak area is more or less the same, wherein of a relatively high with 50%MeOH for Extraction solvent peak area, therefore selects 50%MeOH molten for extracting
Agent.In conjunction with the preparation condition of one Radix Scrophulariae [assay] test sample of " Chinese Pharmacopoeia " version in 2010, because granule is extracted
After material more soluble compared with medical material, extracting mode is supersound extraction, and the time is 30min.
Experimental example 3The foundation of Radix Scrophulariae granule characteristic fingerprint pattern
With reference to " technical manual (trying) of Chinese medicine finger printing research ", Chinese Pharmacopoeia committee is utilized to recommend
" similarity evaluation 2012 editions " software, by carrying out similarity ratio to gained finger printing
Compared with (setting up reference feature finger printing with average), and carry out methodological study.
According to experimental example 1 and 2, determine that Radix Scrophulariae granule HPLC characteristic spectrum is set up as follows:
(1) Radix Scrophulariae granule is taken appropriate, finely ground, take about 0.5g, accurately weighed, put in tool plug conical flask, accurate addition
50% methanol 50mL, close plug, weighed weight, supersound process (power 500W, frequency 40kHz) 30min, let cool, more weighed weight,
Supply the weight of less loss with 50% methanol, shake up, filter, take subsequent filtrate, to obtain final product.
(2) high-efficient liquid phase chromatogram condition: with Agilent Zorbax SB-C18 5 μm, 4.6mm × 250mm (PN:
880975-902) it is chromatographic column；With acetonitrile as mobile phase A, 0.05% phosphoric acid solution is Mobile phase B, carries out gradient by table 8 and washes
De-；Flow velocity 1.0mL/min, column temperature 25 DEG C；Detection wavelength: front 18min is 210nm, is changed to 278nm afterwards.Theoretical cam curve is pressed
Harpagoside calculates should be not less than 5000.Sample size: 10 μ L.
Table 8 gradient elution program
Carry out the foundation of the common pattern of Radix Scrophulariae granule characteristic spectrum as stated above.
Take the Radix Scrophulariae granule sample of 18 batches as need testing solution, obtain Radix Scrophulariae by high performance liquid chromatography and join
Side's particle characteristic collection of illustrative plates, the characteristic spectrum of 18 batches of Radix Scrophulariae granules (S1～S18 be followed successively by lot number A1301044, A1301045,
A1300816、1305369、1305370、1305371、G1306007、G1306008、G1306009、130701、130702、
130703,1303100,1303112,1303124, the figure of the Radix Scrophulariae granule of 1306001S, 1306002S, 1306003S
Spectrum) as it is shown in fig. 7, use committee of pharmacopeia establishment fingerprint similarity evaluation software " chromatographic fingerprints of Chinese materia medica is similar
Degree evaluation system 2012 editions ", the comparison characteristic fingerprint pattern of generation as shown in Figure 8, the testing result to granule characteristic pattern
It is analyzed, compares, choose harpagoside therein as with reference to peak (S peak), when calculating that each characteristic peak is relative with S peak to be retained
Between setting, acquired results is as shown in table 10～12.
Table 10 Radix Scrophulariae granule comparison characteristic fingerprint pattern relative retention time
12 18 batches of Radix Scrophulariae granule similarity result of table
Shown in table 10～12 and Fig. 7～8, each batch with the similarity compareing characteristic fingerprint pattern all more than 0.90.
Experimental example 4Radix Scrophulariae granule characteristic fingerprint pattern Method validation
4.1 precision
4.1.1 repeated experiment
Taking same lot number test sample (lot number 1306001S) 6 parts, empirically the condition of example 3 measures 4 total peaks respectively
Relative retention time, relative retention time result is as shown in table 13, and similarity result is as shown in table 14, chromatogram such as Figure 10 institute
Show.
From table 13～14 and Figure 10, the RSD of the relative retention time at 1～No. 3 peak and object of reference S peak is respectively
0.12%, 0.04%, 0.04%, similarity is respectively 1.00；This shows the repeatability of this method preferably.
Table 13 repeated experiment result
Table 14 repeated experiment similarity result
4.1.2 Precision Experiment
Take with a need testing solution (lot number 1306001S), the empirically chromatographic condition of example 3, repeat sample introduction 6 times, measure
The relative retention time at 4 total peaks, relative retention time result is as shown in Table 15, and similarity result is such as shown in Table 16, color
Spectrogram is as shown in Figure 10.
Table 15 Precision Experiment result
Table 16 Precision Experiment similarity result
From table 15～16 and Figure 10, the RSD of the relative retention time at 1～No. 3 peak and object of reference S peak is respectively
0.12%, 0.03%, 0.03%, similarity is respectively 1.00, and this shows that precision is preferable.
4.2 specificity
This product is the folk prescription granule of Radix Scrophulariae decoction pieces, and the Extraction solvent of test sample is 50% methanol, therefore accurate absorption test sample
The each 10 μ L of solution, negative control solution, are injected separately into high performance liquid chromatograph, and empirically the chromatographic condition of example 3 measures, and result is such as
Shown in Figure 11.As shown in Figure 11, result feminine gender is noiseless.
4.3 ruggedness
Stability of solution is tested
Take same lot number test sample (lot number 1306001S), after preparation, empirically the chromatographic condition of example 3 respectively 0,2,
4,6,12,14,16,18,20,22,24 hours sample introductions, measure the relative retention time at 4 total peaks, relative retention time result
As shown in table 17, similarity result is as shown in table 18, and chromatogram is as shown in figure 12.
Table 17 stability of solution experimental result
Table 18 stability experiment similarity result
From table 17～18 and Figure 12, the RSD of the relative retention time at 1～No. 3 peak and object of reference S peak is respectively
0.21%, 0.02%, 0.05%, similarity is respectively 1.00；This shows the confession obtained by test sample preparation method of the present invention
Test sample solution is stable in 24 hours, and similarity is preferable.
Obviously, above-described embodiment is only for clearly demonstrating example, and not restriction to embodiment.Right
For those of ordinary skill in the field, can also make on the basis of the above description other multi-form change or
Variation.Here without also cannot all of embodiment be given exhaustive.And the obvious change thus extended out or
Change among still in the protection domain of the invention.
Claims (10)
1. the method for the finger printing of the pharmaceutical preparation setting up Radix Scrophulariae, it is characterised in that the method comprises the steps:
(1) the pharmaceutical preparation 0.4-0.6 weight portion of Radix Scrophulariae to be measured is taken, accurately weighed, accurate addition 40～60% methanol aqueous solution
40-60 parts by volume, weighed weight, heating and refluxing extraction or supersound extraction 20-40 minute, let cool, more weighed weight, take 40～
60% methanol aqueous solution supplies the weight of less loss, shakes up, and filters, takes subsequent filtrate, as need testing solution；
(2) precision weighs Harpagide reference substance, adds 40～60% methanol aqueous solution makes every 1 parts by volume containing 0.00004-
The solution of 0.00008 weight portion, shakes up, as reference substance solution A；
Precision weighs harpagoside reference substance, adds 40～60% methanol aqueous solution makes every 1 parts by volume containing 0.00001-0.00003
The solution of weight portion, shakes up, as reference substance B solution；
Precision weighs cinnamic acid reference substance, adds 40～60% methanol aqueous solution makes every 1 parts by volume containing 0.00001-0.00003 weight
The solution of amount part, shakes up, as reference substance C solution；
(3) chromatographic condition: with octadecylsilane chemically bonded silica as filler, the phosphoric acid with acetonitrile as mobile phase A, with 0.05%
Solution is that Mobile phase B carries out gradient elution according to following program: 0-10min, A:B are 5%:95% → 8%:92%；10-
20min, A:B are 8%:92% → 22%:78%；20-25min, A:B are 22%:78% → 27.5%:72.5%；25-
30min, A:B are 27.5%:72.5% → 28%:72%；30-40min, A:B are 28%:72% → 35%:65%；40-
45min, A:B are 35%:65% → 100%:0%；Detection wavelength is 210nm (0～18min) and 278nm (18～45min)；
Column temperature is 25 DEG C, and flow velocity is 1mL/min；
(4) precision draws need testing solution need testing solution, reference substance solution A, reference substance B solution and reference substance C solution respectively
0.010-0.020 parts by volume, inject high performance liquid chromatograph, measure, respectively need testing solution, reference substance solution A and, comparison
Product B solution and the liquid chromatograph of reference substance C solution；
(5) Chinese Pharmacopoeia Commission's similarity evaluation is utilized, to need testing solution, reference substance A
Solution, the liquid chromatograph of reference substance B solution reference substance C solution import respectively through data, and Supplements and Data Matching to obtain final product
Finger printing；
Described weight portion is g/mL with the relation of described parts by volume.
The method of the finger printing of the pharmaceutical preparation setting up Radix Scrophulariae the most according to claim 1, it is characterised in that
The method comprises the steps:
(1) pharmaceutical preparation 0.5 weight portion of Radix Scrophulariae to be measured is taken, accurately weighed, accurate addition 50% methanol aqueous solution 50 parts by volume,
Weighed weight, heating and refluxing extraction or supersound extraction 30 minutes, let cool, more weighed weight, takes 50% methanol aqueous solution and supplies and subtract
The weight lost, shakes up, and filters, takes subsequent filtrate, as need testing solution；
(2) precision weighs Harpagide reference substance, adds 50% methanol aqueous solution and makes molten containing 0.00006 weight portion of every 1 parts by volume
Liquid, shakes up, as reference substance solution A；
Precision weighs harpagoside reference substance, adds 50% methanol aqueous solution and makes molten containing 0.00002 weight portion of every 1 parts by volume
Liquid, shakes up, as reference substance B solution；
Precision weighs cinnamic acid reference substance, adds 40～60% methanol aqueous solution is made every 1 parts by volume and contained the molten of 0.00002 weight portion
Liquid, shakes up, as reference substance C solution；
(3) chromatographic condition: with octadecylsilane chemically bonded silica as filler, the phosphoric acid with acetonitrile as mobile phase A, with 0.05%
Solution is that Mobile phase B carries out gradient elution according to following program: 0-10min, A:B are 5%:95% → 8%:92%；10-
20min, A:B are 8%:92% → 22%:78%；20-25min, A:B are 22%:78% → 27.5%:72.5%；25-
30min, A:B are 27.5%:72.5% → 28%:72%；30-40min, A:B are 28%:72% → 35%:65%；40-
45min, A:B are 35%:65% → 100%:0%；Detection wavelength is 210nm (0～18min) and 278nm (18～45min)；
Column temperature is 25 DEG C, and flow velocity is 1mL/min；
(4) precision draws need testing solution need testing solution, reference substance solution A, reference substance B solution and reference substance C solution respectively
0.015 parts by volume, injects high performance liquid chromatograph, measures, and obtains need testing solution, reference substance solution A, reference substance B solution respectively
Liquid chromatograph with reference substance C solution；
(5) Chinese Pharmacopoeia Commission's similarity evaluation is utilized, to need testing solution, reference substance A
Solution and, the liquid chromatograph of reference substance B solution and reference substance C solution import respectively through data, Supplements and Data Matching,
Obtain finger printing.
The method of the finger printing of the pharmaceutical preparation setting up Radix Scrophulariae the most according to claim 1 and 2, it is characterised in that with
4.6mm × 250mm, Agilent Zorbax SB-C18,4.6mm × 250mm, the Diamonsil C18 of 5 μm of 5 μm or
4.6mm × 250mm, the Shim-pack VP-ODS of 5 μm are chromatographic column.
4., according to the method for the finger printing of the pharmaceutical preparation setting up Radix Scrophulariae described in any one of claim 1-3, its feature exists
In, described pharmaceutical preparation be tablet, capsule, pill, granule, honey refining pill, slow releasing preparation, quick releasing formulation, controlled release preparation,
Oral liquid or ejection preparation.
5., according to the method for the finger printing of the pharmaceutical preparation setting up Radix Scrophulariae described in any one of claim 1-4, its feature exists
In, the pharmaceutical preparation of described Radix Scrophulariae is prepared by the following method and forms:
Take Radix Scrophulariae, heating and refluxing extraction at least 1 time, add the water extraction at least 0.5h of at least 2 weight times amount every time, filter, close
And filtrate, it is 1.10～1.15 that filtrate is concentrated into 60 DEG C of relative densities, adds customary adjuvant, according to common process, makes clinic
Upper acceptable tablet, capsule, pill, granule, honey refining pill, slow releasing preparation, quick releasing formulation, controlled release preparation, oral liquid
Body preparation or ejection preparation.
The method of the finger printing of the pharmaceutical preparation setting up Radix Scrophulariae the most according to claim 5, it is characterised in that described profound
The pharmaceutical preparation of ginseng is prepared by the following method and forms:
Take Radix Scrophulariae, heating and refluxing extraction 1～5 times, add the water extraction 0.5～3.0h of 4～10 weight times amount every time, filter, close
And filtrate, it is 1.10～1.15 that filtrate is concentrated into 60 DEG C of relative densities, adds customary adjuvant, according to common process, makes clinic
Upper acceptable tablet, capsule, pill, granule, honey refining pill, slow releasing preparation, quick releasing formulation, controlled release preparation, oral liquid
Body preparation or ejection preparation.
The method of the finger printing of the pharmaceutical preparation setting up Radix Scrophulariae the most according to claim 6, it is characterised in that described profound
The pharmaceutical preparation of ginseng is prepared by the following method and forms:
Take Radix Scrophulariae, heating and refluxing extraction 2 times, the water extraction 2.0h that the 1st time adds 8 weight times amount, add 6 weight times amount the 2nd time
Water extraction 1.5h, filter, merging filtrate, it is 1.10～1.15 that filtrate is concentrated into 60 DEG C of relative densities, add customary adjuvant, press
More solito technique, makes the most acceptable tablet, capsule, pill, granule, honey refining pill, slow releasing preparation, rapid release system
Agent, controlled release preparation, oral liquid or ejection preparation.
8., according to the method for the finger printing of the pharmaceutical preparation setting up Radix Scrophulariae described in any one of claim 1-7, its feature exists
In, in the finger printing of the pharmaceutical preparation of described Radix Scrophulariae, common characteristic peak is: S peak harpagoside, No. 1 peak Harpagide, No. 2 peaks
With No. 3 peak cinnamic acid, with S peak harpagoside for internal reference peak, each peak relative retention time be respectively as follows: No. 1 peak 0.22～
0.26, No. 2 peaks 0.75～0.89, S peak 1.00 and No. 3 peaks 1.06～1.24.
9., according to the method for the finger printing of the pharmaceutical preparation setting up Radix Scrophulariae described in any one of claim 1-8, its feature exists
In, in the finger printing of the pharmaceutical preparation of described Radix Scrophulariae, each peak relative retention time is respectively as follows: peak, No. 1 peak 0.24,2
0.82, S peak 1.00 and No. 3 peaks 1.15.
10. the answering in the quality testing and quality control of the pharmaceutical preparation of Radix Scrophulariae of the method described in any one of claim 1-9
With.
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| CN107271598A (en) * | 2017-07-20 | 2017-10-20 | 青岛市食品药品检验研究院 | The construction method of Chinese patent drug Yanyan slice standard feature collection of illustrative plates and application |
| CN107607653A (en) * | 2017-11-08 | 2018-01-19 | 扬子江药业集团有限公司 | The method for determining Radix Scrophulariae extract finger-print |
| CN107807187A (en) * | 2017-10-27 | 2018-03-16 | 天圣制药集团股份有限公司 | Method that is a kind of while determining harpagide in radix scrophulariae, harpagoside and cinnamic acid |
| CN107907602A (en) * | 2017-10-27 | 2018-04-13 | 天圣制药集团股份有限公司 | A kind of construction method of radix scrophulariae finger-print |
| CN109709249A (en) * | 2018-12-27 | 2019-05-03 | 药圣堂（湖南）制药有限公司 | A kind of Quality evaluation method based on the more active component detections of radix scrophulariae |
| CN110960596A (en) * | 2019-12-29 | 2020-04-07 | 贵州中医药大学 | Radix scrophulariae producing area processing and concocting integrated preparation process and detection method |
| CN112710759A (en) * | 2021-03-29 | 2021-04-27 | 江西省药品检验检测研究院 | Quality detection method of Mailuoning granules |
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| CN107271598A (en) * | 2017-07-20 | 2017-10-20 | 青岛市食品药品检验研究院 | The construction method of Chinese patent drug Yanyan slice standard feature collection of illustrative plates and application |
| CN107807187A (en) * | 2017-10-27 | 2018-03-16 | 天圣制药集团股份有限公司 | Method that is a kind of while determining harpagide in radix scrophulariae, harpagoside and cinnamic acid |
| CN107907602A (en) * | 2017-10-27 | 2018-04-13 | 天圣制药集团股份有限公司 | A kind of construction method of radix scrophulariae finger-print |
| CN107607653A (en) * | 2017-11-08 | 2018-01-19 | 扬子江药业集团有限公司 | The method for determining Radix Scrophulariae extract finger-print |
| CN109709249A (en) * | 2018-12-27 | 2019-05-03 | 药圣堂（湖南）制药有限公司 | A kind of Quality evaluation method based on the more active component detections of radix scrophulariae |
| CN110960596A (en) * | 2019-12-29 | 2020-04-07 | 贵州中医药大学 | Radix scrophulariae producing area processing and concocting integrated preparation process and detection method |
| CN112710759A (en) * | 2021-03-29 | 2021-04-27 | 江西省药品检验检测研究院 | Quality detection method of Mailuoning granules |
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