CN107389827A - The assay method of stachydrine hydrochloride content in motherwort or its compound preparation - Google Patents
The assay method of stachydrine hydrochloride content in motherwort or its compound preparation Download PDFInfo
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- CN107389827A CN107389827A CN201710713169.5A CN201710713169A CN107389827A CN 107389827 A CN107389827 A CN 107389827A CN 201710713169 A CN201710713169 A CN 201710713169A CN 107389827 A CN107389827 A CN 107389827A
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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
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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Abstract
The present invention relates to stachydrine hydrochloride assay technical field, the assay method of stachydrine hydrochloride content in more particularly to a kind of motherwort or its compound preparation：Test sample sour regulation system pH value to 1~2 is treated, mixed type cation exchange solid-phase extraction column is crossed and is eluted successively with water, methanol, then is eluted by several times with dense ammonia alcoholic solution, eluent is collected, obtains testing sample, detect.The method of the present invention quickly, conveniently, good separating effect, can accurately obtain object, and stability is good, high sensitivity, and testing result is accurate.
Description
Technical field
The present invention relates to stachydrine hydrochloride assay technical field, in more particularly to a kind of motherwort or its compound preparation
The assay method of stachydrine hydrochloride content.
Background technology
Motherwort is labiate motherwort Leonurus ja ponicus Houtt. aerial part.In conventional
Medicine, acrid flavour is bitter, cool, invigorates blood circulation, silt of dispelling, menstruation regulating, disappear water, treats menoxenia, threatened abortion difficult labour, placenta retension, postpartum anemic fainting,
Abdominal pain due to blood stasis, metrorrhagia and metrostaxis, hematuria, rush down blood, carbuncle swells sore.Due to its inducing diuresis to remove edema, shrink uterus effect significantly, be successive dynasties doctor
Family is used for treating the key medicine of gynaecological disease.
Stachydrine hydrochloride, chemical name：(S)-2-carboxy-1,1-dimethylpyrrolidinium chloride；Point
Minor：C7H13NO2·HCl；Molecular weight:179.5；No. CAS：471-87-4.
Stachydrine hydrochloride is white waxy solid, is mainly derived from the leaf of motherwort, can improve coronary artery and cardiac muscle is sought
Nourish one's nature CBF, reduce myocardium cell necrosis amounts, reduce vascular resistence, improve microcirculation, reducing heart rate, reduce cardiac output etc.
Effect (is expected to the medicine as good disease of cardiovascular system)；The generation of breast cancer and endometriosis interna can be suppressed；
There is eliminating the phlegm, antibechic, relaxation bronchial smooth muscle；Also there is the contraction frequency for slowing down the frog heart, dog, rabbit can be reduced out
Blood rate and bleeding time, excited uterus etc. act on.Because pharmacological action is clear and definite, and content is higher, always as index composition
For carrying out quality control to motherwort and its compound preparation.
In the prior art, the preprocess method on stachydrine hydrochloride assay mainly includes the Reinecke's salt precipitation method, strong
Polarity cation exchange resin, methanol (ethanol) direct extraction method, C18 solid phase extraction column methods of purification etc..
The Reinecke's salt precipitation method be traditional classical stachydrine hydrochloride assay method, this method operation it is extremely cumbersome, it is necessary to through
It is poor to cross process, the accuracys such as precipitation repeatedly, dissolving.Limitation of the highly polar cation exchange resin due to ion exchange resin in itself
Property can not realize commercialization, it is necessary to by hand dress post, influence factor is more, and reappearance can not ensure, and reagent dosage is excessive, expend
Time is grown.
Methanol (ethanol) direct extraction method and the C18 solid phase extraction column methods of purification, operation is relatively easy, but for Chinese medicine
Compound preparation, because component content is more, it can not often realize being kept completely separate for multiple chromatographic peaks.Such as public affairs in CN105911187A
The method of stachydrine hydrochloride content in a kind of liquid matter Series detectors tablet for women's health and tranquilness opened, 1) this product 10 is taken, coating is removed, it is accurate
It is weighed, it is finely ground, about 2g is taken, it is accurately weighed, put in conical flask, precision adds 80% ethanol 20ml, close plug, weighed weight, ultrasound
30min is extracted, is let cool, then weighed weight, the weight of less loss is supplied with 80% ethanol, is shaken up, difference is passed through with 1ml/min flow velocitys
The C18 solid phase extraction columns activated with 3ml ethanol and 3ml water, with 5ml water wash, are discarded, then are collected and washed with 5ml ethanol elutions
De- liquid, eluent nitrogen at 40 DEG C, which is blown to, closely to be done, and precision adds the dissolving of 1ml ethanol, with 0.22 μm of organic membrane filtration, takes continuous filter
Liquid, produce need testing solution；2) the scarce motherwort negative sample in prescription ratio and technique preparation is taken, by the system of need testing solution
Preparation Method prepares negative control solution；3) accurately weighed stachydrine hydrochloride reference substance 17.42mg, into 25ml measuring bottles, adds methanol
The hydrochloric stachydrine 0.6940mg of every 1ml solution is diluted to, precision draws 5ml, adds methanol dilution to obtain every 1ml to 25ml and contain
Stachydrine hydrochloride 0.1388mg reference substance solution；4) need testing solution, reference substance solution and negative control solution are taken respectively, are used
The triple level Four bar liquid chromatography mass spectrometric combined instrument detections of Agilent1295-6550C.The method needs to be examined using mass detector
Survey, common liquid chromatography does not reach being kept completely separate for chromatographic peak, and testing cost is higher.
For another example the method disclosed in CN 105548424A, (HPLC-ELSD methods) sample direct injected after processing detect,
Calculated using reference substance external standard two-point method logarithmic equation.Peak area, concentration are in good linear relationship after taking the logarithm respectively, lack benefit
Brittle Falsepimpernel Herb negative control is noiseless, and each peak separating degree is good.It is the stability of solution of this method, precision, repeatability, the degree of accuracy, resistance to
It is good with the more original thin layer chromatography scanning of property (TLCS), but for multi-component compound Chinese medicinal preparation, multiple chromatograms can not be realized
Peak is kept completely separate, and the scope of application is small.
The content of the invention
In order to solve present in above prior art, accuracy is poor, chromatographic peak complete in stachydrine hydrochloride assay
The problem of difficult is separated, the invention provides a kind of easy to operate, can accurately obtain object, and stability is good, high sensitivity, inspection
Survey the assay method of stachydrine hydrochloride content in the accurate motherwort of result or its compound preparation.
For the stachydrine hydrochloride in Precision measurement compound preparation, carried out for the preprocess method of motherwort compound preparation
A large amount of and in-depth study, in research process, inventor has found：Compound preparation composition and its contains compared with single preparations of ephedrine
Measure increasingly complex, only apply mechanically the preprocess method of stachydrine hydrochloride in motherwort, accurately and effectively can not extract and detect
Stachydrine hydrochloride in compound preparation.Subject matter is that chemical composition is excessive in compound preparation, chromatographic peak mistake in sample chromatogram
More, chromatographic peak separating degree is poor.
Found after further investigation：Compound preparation is dissolved in specific solvent, by specific processing method, passed through
Specific separation method, obtained material can detect to obtain by HPLC ELSD detector, and detect
The degree of accuracy, precision, repeatability and other effects it is excellent.
The present invention is achieved by the following measures：
The assay method of stachydrine hydrochloride content in a kind of motherwort or its compound preparation, (1) is by motherwort or its compound
Solid pharmaceutical preparation is after alcohol extracting, or motherwort or its compound liquid preparation, with sour regulation system pH value to 1~2, centrifuges,
Supernatant is taken, is added on mixed type cation exchange solid-phase extraction column, is eluted successively with water, methanol, is discarded eluent, reuse
Certain density dense ammonia alcoholic solution elutes by several times, collects eluent, steams to without ammonia taste, with alcohol constant volume, filtering, produces and treat test sample
Product, (2) are used the chromatographic column using propyl amides bonded silica gel as filler, detected using EISD, with
Second order logarithmic equation calculates the amount of stachydrine hydrochloride in testing sample, further calculates hydrochloric acid water in motherwort or its compound preparation
The content of Soviet Union's alkali.It is preferred that dense ammonia alcoholic solution concentration is 20-30%.
Those skilled in the art understand：Compound preparation refers to two or more medicine mix preparation.The present invention
Described motherwort compound preparation refers to the composition material medicine containing motherwort, routinely technique, adds customary adjuvant and prepares
Into clinically-acceptable any formulation, the motherwort or its compound solid preparation include pill, powder, granule, piece
Agent, lozenge, soft extract, emplastrum, pill, capsule, liquid extract and extract, plaster, gel, ointment, film
Agent, suppository, nasal formulations or eye-drops preparations；Motherwort or its compound liquid preparation include syrup, mixture, tincture, liniment, wine
Agent, injection, lotion, aerosol, nasal formulations, eye-drops preparations or spray.
With the glacial acetic acid solution of acetonitrile -0.2% (80: 20) for mobile phase in preferred steps (2).
With 0.5mol/L hydrochloric acid solutions regulation pH in preferred steps (1).
20% dense methanolic ammonia solution 10ml is eluted by several times in preferred steps (1).
According to currently preferred, a kind of bulk drug composition is motherwort 150g, Radix Angelicae Sinensis 150g, radix paeoniae rubrathe 150g, the red sage root
150g, root tuber of aromatic turmeric 100g, root of bidentate achyranthes 150g, Fructus Aurantii 100g, banksia rose 50g, charred schizonepeta 100g, ginger charcoal 50g, madder 100g, total amount is made
The preprocess method of stachydrine hydrochloride, step are as follows in the 1000ml female peaceful oral liquid of compound Chinese medicinal preparation：
Precision measures this product 5ml, puts in 10ml volumetric flasks, is 1 with 0.5mol/L hydrochloric acid solutions regulation pH value, is diluted with water
To scale, shake up, centrifugation (5000 revs/min) 5 minutes, take supernatant 1ml, be added in commercially available mixed type cation exchange solid phase extraction
Take on post (6cc/500mg, being pre-processed respectively with each 6ml of first alcohol and water), eluted successively with water, each 6ml of methanol, discard elution
Liquid, then 20% dense methanolic ammonia solution 10ml are eluted by several times, collect eluent, steam to without ammonia taste, 5ml amounts are transferred to proper amount of methanol
In bottle, and scale is diluted to, shakes up, produce.
According to currently preferred, a kind of bulk drug composition is motherwort 2200g, prepared rhizome of rehmannia 275, Radix Angelicae Sinensis 825g, is made
The preprocess method of stachydrine hydrochloride, step are as follows in total amount 1000g compound Chinese medicinal preparation Compound Prescribe Motherwort Herb Capusle：
Take this product appropriate, mix, finely ground, precision weighs 0.5g, puts in conical flask with cover, and precision adds 70% ethanol
25ml, weighed weight, it is heated to reflux 2 hours, lets cool, then weighed weight, the weight of less loss is supplied with 70% ethanol, is shaken up, is filtered
Cross, take subsequent filtrate, precision measures 2ml, puts in 10ml volumetric flasks, is 1 with 0.5mol/L hydrochloric acid solutions regulation pH value, is diluted with water
To scale, shake up, centrifugation (5000 revs/min) 5 minutes, take supernatant 1ml, be added in commercially available mixed type cation exchange solid phase extraction
Take on post (6cc/150mg, being pre-processed respectively with each 6ml of first alcohol and water), eluted successively with water, each 6ml of methanol, discard elution
Liquid, then 30% dense methanolic ammonia solution 10ml are eluted by several times, collect eluent, steam to without ammonia taste, 5ml amounts are transferred to proper amount of methanol
In bottle, and scale is diluted to, shakes up, produce.
Beneficial effects of the present invention：
The preprocess method of the present invention quickly, conveniently, good separating effect, can accurately obtain object, and stability is good, spirit
Sensitivity is high, and testing result is accurate.
Brief description of the drawings：
Reference substance high-efficient liquid phase chromatogram in Fig. 1 test examples 1；
Test sample uses the high-efficient liquid phase chromatogram that the inventive method obtains in Fig. 2 test examples 1；
Motherwort feminine gender high-efficient liquid phase chromatogram in Fig. 3 test examples 1；
Reference substance high-efficient liquid phase chromatogram in Fig. 4 test examples 2；
Test sample uses the high-efficient liquid phase chromatogram that the inventive method obtains in Fig. 5 test examples 2；
Motherwort feminine gender high-efficient liquid phase chromatogram in Fig. 6 test examples 2.
Embodiment
Detailed elaboration is made to the present invention with reference to embodiment, but is not limited to these embodiments specifically recorded.
Embodiment 1
1. instrument, reagent and test sample
The high performance liquid chromatographs of Agilent 1200 (including G1322A degassers, G1311A quaternary pumps, G1329A enter automatically
Sample device, G1316A column ovens, 380ELSD detectors, ChemStation work stations)；Sartorius CP225D electronic balances
(German Sai Duolisi groups).
Reference substance：Stachydrine hydrochloride, purchased from National Institute for Food and Drugs Control, lot number：110712-201513；
In addition to acetonitrile is chromatographically pure, other reagents are pure to analyze.
Testing sample：Female peaceful oral liquid, Rongchang Pharmaceutical (Zibo) Co., Ltd..
2. testing conditions
JADE-PAK Amide chromatographic columns；With the glacial acetic acid solution of acetonitrile -0.2% (80: 20) for mobile phase；Dissipated with evaporative light
Penetrate detector detection.
3. the preparation of reference substance solution
Precision weighs stachydrine hydrochloride reference substance 13.34mg, puts in 25ml measuring bottles, adds methanol to dissolve and is diluted to scale,
Shake up, measure 3ml to the reference substance concentrated solution that concentration is 0.5336mg/ml, then precision, put in 10ml measuring bottles, add methanol dilution
To scale, shake up, that is, obtain the reference substance solution that concentration is 0.1601mg/ml.
4. the preparation of need testing solution
The selection of 4.1SPE fillers
Respectively with commercially available mixed type cation exchange solid-phase extraction column, mixed type anion-exchange solid phase extraction post, mixing
Type weak cation exchange solid-phase extraction column, mixed type weak anionic exchange solid-phase extraction column, are tested, as a result only mixed type
Cation exchange solid-phase extraction column has absorption to stachydrine hydrochloride, can be used for the measure of the composition.
The investigation of 4.2SPE eluting solvents
After have selected mixed type cation exchange solid-phase extraction column, further eluting solvent is investigated.Successively with water,
The dense methanolic ammonia solution of methanol, series concentration (5%, 10%, 15%, 20%, 25%) is tested, find using water and methanol as
During eluting solvent, stachydrine hydrochloride can be retained on SPE posts, will not be eluted, and can be used for water-soluble in removal testing sample
Property and alcohol dissolubility impurity；Stachydrine hydrochloride can be submitted to change clothes and taken off by dense ammonia methanol from SPE posts, compare the dense of various concentrations
Methanolic ammonia solution, when dense ammonia content reaches more than 15%, the basic indifference of measurement result, in order to ensure to elute effect, it will elute
Solvent is defined as 20% dense methanolic ammonia solution.
The investigation of 4.3 solvent elution amounts
The elution effect that elution amount is 6ml, 8ml, 10ml is investigated respectively, it is found that when solvent elution amount reaches more than 6ml, is washed
The basic indifference of de- effect, in order to ensure to elute effect, solvent elution amount is determined into 10ml.
The investigation of 4.4SPE column capacitys
Investigate commercially available 3cc, 60mg, 6cc respectively, 150mg, 6cc, 500mg, 20cc, 1000mg difference column capacity SPE posts
Effect, for this kind, column capacity reaches 500mg can ensure experimental result substantially.
The preparation method of final determination need testing solution is as follows：Precision measures this product 5ml, puts in 10ml volumetric flasks, uses
0.5mol/L hydrochloric acid solutions are diluted to scale (pH value is 1~2), shake up, centrifugation (5000 revs/min) 5 minutes, take supernatant
1ml, it is added in commercially available mixed type cation exchange solid-phase extraction column (6cc/500mg, being pre-processed respectively with each 6ml of first alcohol and water)
On, eluted successively with water, each 6ml of methanol, discard eluent, then 20% dense methanolic ammonia solution 10ml is eluted by several times, collects elution
Liquid, steam extremely without ammonia taste, be transferred to proper amount of methanol in 5ml measuring bottles, and be diluted to scale, shake up, produce.
5. the investigation of standard curve and linear relationship
Precision draws each 1,2,5,10,15,20 μ l of reference substance solution under " 3 " item.Liquid chromatograph is injected, is determined respectively
Integrating peak areas value.Using the logarithm value of reference substance sample size as abscissa, the logarithm value of integrating peak areas value is ordinate, is carried out
Linear regression, obtain regression equation.Measurement result is shown in Table 1.
The stachydrine hydrochloride linear relationship of table 1 investigates result
Regression equation y=1.2509x+5.6881, correlation coefficient r=0.9998.
Result of the test shows, the logarithm value and peak of stachydrine hydrochloride sample size sample size between 0.3202~3.2020 μ g
The logarithm value of area integral value is in good linear relationship.
6. precision test
Precision draws the μ l of reference substance solution 15 under " 3 " item, injects liquid chromatograph, METHOD FOR CONTINUOUS DETERMINATION 6 times, record peak area is simultaneously
The relative standard deviation (RSD) of its logarithm value is calculated, the results are shown in Table 2.Show that instrument precision is good.
The Precision test result of table 2
7. stability test
Precision draws same need testing solution, distinguishes the μ l of sample introduction 20 in 0,5,10,15,20,25h, records peak area, calculate
The relative standard deviation (RSD) of peak area logarithm value, the results are shown in Table 3.It is substantially steady in 25h to show that composition to be measured is placed in room temperature
It is fixed.
The stability test result of table 3
8. replica test
Same sample is taken, replication 6 times, content is calculated, the results are shown in Table 4.Show that analysis method repeatability is good.
The replica test result of table 4
9. recovery test
6 parts of the sample that content has been predicted under " 8 " item is taken, every part of 2.5ml, is put in 10ml measuring bottles, it is accurate respectively to add equivalent
Reference substance, by legal system available test sample solution below " 3 " item.Distinguish the μ l of sample introduction 20 by above-mentioned chromatographic condition, calculate the rate of recovery, as a result
It is shown in Table 5.Show that the rate of recovery of this method is good.
The rate of recovery experimental result of table 5
Test example 1：
A kind of bulk drug composition is motherwort 150g, Radix Angelicae Sinensis 150g, radix paeoniae rubrathe 150g, red sage root 150g, root tuber of aromatic turmeric 100g, the root of bidentate achyranthes
150g, Fructus Aurantii 100g, banksia rose 50g, charred schizonepeta 100g, ginger charcoal 50g, madder 100g, total amount 1000ml Chinese medicine compound prescription system is made
The female peaceful oral liquid of agent, the assay method of wherein stachydrine hydrochloride content are as follows：
Chromatographic condition and system suitability：Using propyl amides bonded silica gel as filler；With the ice vinegar of acetonitrile -0.2%
Acid solution (80: 20) is mobile phase；Detected with EISD.
The preparation of reference substance solution：Take stachydrine hydrochloride reference substance appropriate, it is accurately weighed, add methanol that every 1ml is made and contain
0.15mg solution, is produced.
The preparation of need testing solution：Precision measures this product 5ml, puts in 10ml volumetric flasks, is adjusted with 0.5mol/L hydrochloric acid solutions
It is 1 to save pH value, is diluted with water to scale, shakes up, and centrifugation (5000 revs/min) 5 minutes, takes supernatant 1ml, is added in commercially available mixing
It is each with water, methanol successively on type cation exchange solid-phase extraction column (6cc/500mg, being pre-processed respectively with each 6ml of first alcohol and water)
6ml is eluted, and discards eluent, then 20% dense methanolic ammonia solution 10ml is eluted by several times, collects eluent, is steamed to without ammonia taste, with suitable
Amount methanol is transferred in 5ml measuring bottles, and is diluted to scale, is shaken up, is produced.
Determination method：It is accurate respectively to draw μ l of reference substance solution 5,15 μ l, the μ l of need testing solution 10~20, inject liquid chromatogram
Instrument, measure, calculated, produced with external standard two-point method logarithmic equation.
As a result three batches of test sample measurement results are respectively 0.67mg/ml, 0.55mg/ml, 0.60mg/ml.Typical chromatogram
Figure is shown in the stachydrine hydrochloride reference substance of accompanying drawing 1, the need testing solution of accompanying drawing 2, the negative sample of accompanying drawing 3 respectively.
Test example 2：
A kind of bulk drug composition is motherwort 2200g, prepared rhizome of rehmannia 275, Radix Angelicae Sinensis 825g, and the Chinese medicine that total amount 1000g is made is answered
The preprocess method of stachydrine hydrochloride, step are as follows in square preparation Compound Prescribe Motherwort Herb Capusle：
Chromatographic condition and system suitability：Using propyl amides bonded silica gel as filler；With the ice vinegar of acetonitrile -0.2%
Acid solution (80: 20) is mobile phase；Detected with EISD.
The preparation of reference substance solution：Take stachydrine hydrochloride reference substance appropriate, it is accurately weighed, add methanol that every 1ml is made and contain
0.15mg solution, is produced.
The preparation of need testing solution：Take this product appropriate, mix, finely ground, precision weighs 0.5g, puts in conical flask with cover, essence
70% ethanol 25ml of close addition, weighed weight, is heated to reflux 2 hours, lets cool, then weighed weight, and less loss is supplied with 70% ethanol
Weight, shake up, filter, take subsequent filtrate, precision measures 2ml, puts in 10ml volumetric flasks, with 0.5mol/L hydrochloric acid solutions adjust pH
It is worth for 1, is diluted with water to scale, shakes up, centrifugation (5000 revs/min) 5 minutes, take supernatant 1ml, is added in commercially available mixed type sun
On Ion Exchange Solid Phase extraction column (6cc/150mg, being pre-processed respectively with each 6ml of first alcohol and water), successively with water, each 6ml of methanol
Elute, discard eluent, then 30% dense methanolic ammonia solution 10ml is eluted by several times, is collected eluent, is steamed extremely without ammonia taste, with appropriate first
Alcohol is transferred in 5ml measuring bottles, and is diluted to scale, is shaken up, and is produced.
Determination method：It is accurate respectively to draw μ l of reference substance solution 5,15 μ l, the μ l of need testing solution 10~20, inject liquid chromatogram
Instrument, measure, calculated, produced with external standard two-point method logarithmic equation.
As a result three batches of test sample measurement results are respectively 4.1mg/ grains, 4.3mg/ grains, 4.2mg/ grains.Typical chromatogram point
The stachydrine hydrochloride reference substance of accompanying drawing 4, the need testing solution of accompanying drawing 5, the negative sample of accompanying drawing 6 are not seen.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not limited by embodiment
System, it is other it is any without departing from the present invention Spirit Essences with made under principle change, modification, combine, replacement, simplification should be
Equivalence replacement mode, is included within protection scope of the present invention.
Claims (7)
- A kind of 1. assay method of stachydrine hydrochloride content in motherwort or its compound preparation, it is characterised in that（1）By motherwort or its compound solid preparation after alcohol extracting, or motherwort or its compound liquid preparation, adjusted with acid System pH is saved to 1~2, centrifugation, supernatant is taken, is added on mixed type cation exchange solid-phase extraction column, successively with water, methanol Elution, discards eluent, reuses certain density dense ammonia alcoholic solution and elutes by several times, collects eluent, steam to without ammonia taste, use alcohol Constant volume, filtering, produces testing sample,(2) chromatographic column using propyl amides bonded silica gel as filler is used, is detected using EISD, with Second order logarithmic equation calculates the amount of stachydrine hydrochloride in testing sample, further calculates hydrochloric acid water in motherwort or its compound preparation The content of Soviet Union's alkali.
- 2. assay method according to claim 1, it is characterised in that dense ammonia alcoholic solution concentration is 20-30%.
- 3. assay method according to claim 1, it is characterised in that the motherwort or its compound solid preparation include ball Agent, powder, granule, tablet, lozenge, soft extract, emplastrum, pill, capsule, liquid extract and extract, plaster, coagulate Jelly, ointment, plastics, suppository, nasal formulations or eye-drops preparations；Motherwort or its compound liquid preparation include syrup, Mixture, tincture, liniment, vina, injection, lotion, aerosol, nasal formulations, eye-drops preparations or spray.
- 4. assay method according to claim 1, it is characterised in that step（2）In with the glacial acetic acid solution of acetonitrile -0.2%（80 ∶20）For mobile phase.
- 5. assay method according to claim 1, it is characterised in that step（1）It is middle to be adjusted with 0.5mol/L hydrochloric acid solutions pH。
- 6. assay method according to claim 1, it is characterised in that step（1）In 20% dense methanolic ammonia solution 10ml by several times Elution.
- 7. assay method according to claim 1, it is characterised in that step（1）Motherwort or its compound solid preparation are passed through After crossing alcohol extracting, or motherwort or its compound liquid preparation 5ml, put in 10ml volumetric flasks, adjusted with 0.5mol/L hydrochloric acid solutions It is 1 to save pH value, is diluted with water to scale, shakes up, and centrifuges 5 minutes, takes supernatant 1ml, be added in commercially available mixed type cation exchange Solid-phase extraction column（6cc/500mg, pre-processed respectively with each 6ml of first alcohol and water）On, eluted, discarded with water, each 6ml of methanol successively Eluent, then 20% dense methanolic ammonia solution 10ml are eluted by several times, collect eluent, steam to without ammonia taste, 5ml amounts are transferred to methanol In bottle, and scale is diluted to, shaken up, filtered, produce testing sample.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110208417A (en) * | 2019-06-25 | 2019-09-06 | 江西济民可信药业有限公司 | A kind of identification method of high-quality motherwort |
| CN112198274A (en) * | 2020-11-02 | 2021-01-08 | 北京市理化分析测试中心 | Method for detecting pseudoephedrine hydrochloride in paracetamol and pseudoephedrine hydrochloride tablet |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101474249A (en) * | 2009-01-19 | 2009-07-08 | 广西汇科药物研究有限责任公司 | Motherwort and quality control method of preparation thereof |
| CN105548424A (en) * | 2016-01-28 | 2016-05-04 | 南京柯菲平盛辉制药有限公司 | Method for determining content of main active ingredient stachydrine hydrochloride in Naomaili granules and application of main active ingredient stachydrine hydrochloride in Naomaili granules |
| CN105974038A (en) * | 2016-06-24 | 2016-09-28 | 广西灵峰药业有限公司 | Production quality control method of sucrose-free herba leonuri granules |
-
2017
- 2017-08-18 CN CN201710713169.5A patent/CN107389827A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101474249A (en) * | 2009-01-19 | 2009-07-08 | 广西汇科药物研究有限责任公司 | Motherwort and quality control method of preparation thereof |
| CN105548424A (en) * | 2016-01-28 | 2016-05-04 | 南京柯菲平盛辉制药有限公司 | Method for determining content of main active ingredient stachydrine hydrochloride in Naomaili granules and application of main active ingredient stachydrine hydrochloride in Naomaili granules |
| CN105974038A (en) * | 2016-06-24 | 2016-09-28 | 广西灵峰药业有限公司 | Production quality control method of sucrose-free herba leonuri granules |
Non-Patent Citations (3)
| Title |
|---|
| BAOHONG LI 等: "Simultaneous determination and pharmacokinetic study of stachydrine and leonurine in rat plasma after oral administration of Herba Leonuri extract by LC–MS/MS", 《JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS》 * |
| 张晓萍 等: "前列泰丸的质量分析研究", 《中成药》 * |
| 李建芳 等: "HPLC法测定益母草膏中盐酸水苏碱的含量", 《广西中医学院学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110208417A (en) * | 2019-06-25 | 2019-09-06 | 江西济民可信药业有限公司 | A kind of identification method of high-quality motherwort |
| CN112198274A (en) * | 2020-11-02 | 2021-01-08 | 北京市理化分析测试中心 | Method for detecting pseudoephedrine hydrochloride in paracetamol and pseudoephedrine hydrochloride tablet |
| CN112198274B (en) * | 2020-11-02 | 2022-04-05 | 北京市理化分析测试中心 | Method for detecting pseudoephedrine hydrochloride in paracetamol and pseudoephedrine hydrochloride tablet |
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Application publication date: 20171124 |