CN108375646A - A kind of oxalic detection method - Google Patents
A kind of oxalic detection method Download PDFInfo
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- CN108375646A CN108375646A CN201810101833.5A CN201810101833A CN108375646A CN 108375646 A CN108375646 A CN 108375646A CN 201810101833 A CN201810101833 A CN 201810101833A CN 108375646 A CN108375646 A CN 108375646A
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Abstract
The invention discloses a kind of oxalic detection method, this method includes the content assaying method of discrimination method and Saponaretin；The discrimination method and Saponaretin content assaying method result of the detection method are accurate, and high sensitivity is reproducible, as a result reliably, can effectively control oxalic quality, it is ensured that oxalic drug effect.
Description
Technical field
The present invention relates to a kind of oxalic detection methods, belong to the field of drug technology.
Background technology
Creeping oxalis is the fresh of oxalidaceae plant creeping oxalis (Oxalis corniculata L.) or dry herb, is begun
It is loaded in《Compendium of Materia Medica》Also known as Sorrel, three folic acid, ringdove acid, China be distributed mainly on North China, Central China, south China, Jiangxi,
The ground such as Yunnan, Sichuan, it is especially resourceful in Guizhou.It records in version in 2003《Guizhou Province's Chinese medicine, Ethnic crude drugs quality mark
It is accurate》, it is Miao ethnic group of Guizhou Province medicinal herbs most in use.With work(such as clearing heat and detoxicating, Sweeling-eliminating medicine powder disease, tonifying lung purging the liver of pathogenic fire, stomach invigorating cough-relieving, cooling blood and removing stasis
Effect, it is civil to be usually used in treating diarrhea, dysentery, jaundice, gonorrhoea, measles, haematemesis, carbuncle swells, boil, mange, haemorrhoids, rectal prolapse, menstruation
The diseases such as uncomfortable, traumatic injury.Modern pharmacological studies have shown that there is creeping oxalis preferable anti-inflammatory, antiviral, antibacterial and antioxygen to be turned into
With.Currently, the primary formulation containing creeping oxalis medicinal material has：Leaching capsule is secreted, leaching particle is secreted, secretes leaching clearing capsule, FUYANXIAO JIAONANG, six
The multiple peaceful tincture of taste wound, swelling and pain easypro spray, Gukang capsule etc., creeping oxalis is the important Ethnic crude drugs in Guizhou Province.
The quality of Chinese medicine directly affected the clinical efficacy and drug safety of Chinese medicine, in version in 2003《Guizhou Province's Chinese medicine, the people
Race's quality of medicinal material standard》Middle creeping oxalis quality standard only has character description and thin layer discrimination test, and quality standard is simple, cannot
The quality control requirement for meeting the Chinese medicine modern times, for ensure the clinical application of creeping oxalis medicinal material and its preparation safely, effectively, quality can
Control, we study creeping oxalis quality of medicinal material standard, to promote the quality control evaluation method of its medicinal material, for the medicinal material
Research, application, exploitation provide basis.Therefore the present invention carries out system research to oxalic method of quality control, to promote jealous woman
The quality standard of slurry grass lays the foundation, in order to preferably control oxalic quality, it is ensured that drug effect, the present invention provides creeping oxalis
Detection method.
Invention content
The object of the present invention is to provide a kind of oxalic detection methods；The discrimination method of the detection method and different male
Chaste tree glycosides content assaying method result is accurate, and high sensitivity is reproducible, as a result reliably, can effectively control oxalic quality, really
Protect oxalic drug effect.
In order to solve the above technical problems, the present invention adopts the following technical scheme that realization：A kind of oxalic detection method, packet
Include the content assaying method of discrimination method and Saponaretin.
In oxalic detection method above-mentioned, the discrimination method is：Take this product 0.1~1g of powder, add methanol 5~
15ml is ultrasonically treated 10~50 minutes, and filtration takes filtrate as test solution；Creeping oxalis control medicinal material 0.5g separately is taken, adds first
5~15ml of alcohol is ultrasonically treated 10~50 minutes, and filtration takes filtrate medicinal material solution as a contrast；According to《Chinese Pharmacopoeia》Thin-layer chromatography
Method is tested, and each 1~8 μ l of above two solution are drawn, and is put respectively on same silica G plate, with chloroform：Methanol：Formic acid=5
~10：0.5~1.5：0.05~0.15 is solvent, is unfolded, takes out, dry, set and inspected under 360~370nm ultraviolet lamps；For
In test product chromatography, on position corresponding with control medicinal material chromatography, the fluorescence spot of same color is shown.
In oxalic detection method above-mentioned, the discrimination method is：This product powder 0.5g is taken, methanol 10ml is added, is surpassed
Sonication 30 minutes, filtration, takes filtrate as test solution；Creeping oxalis control medicinal material 0.5g separately is taken, adds methanol 10ml, ultrasound
Processing 30 minutes, filtration, takes filtrate medicinal material solution as a contrast；According to《Chinese Pharmacopoeia》Thin-layered chromatography is tested, and draws above-mentioned two
Kind of each 5 μ l of solution are put respectively on same silica G plate, with chloroform-methyl alcohol-formic acid=8：1：0.1 is solvent, expansion,
It takes out, dries, set and inspected under 365nm ultraviolet lamps；In test sample chromatography, on position corresponding with control medicinal material chromatography, show
The fluorescence spot of same color.
In oxalic detection method above-mentioned, the content assaying method of the Saponaretin is：
According to《Chinese Pharmacopoeia》High effective liquid chromatography for measuring；
Chromatographic condition and system suitability：Using octadecylsilane chemically bonded silica as filler；With acetonitrile：0.1%
Phosphoric acid solution=10~20：90~80 be mobile phase；Detection wavelength is 330~340nm；Number of theoretical plate is calculated by Saponaretin peak
Not less than 5000；
The preparation of reference substance solution：Take Saponaretin reference substance appropriate, it is accurately weighed, add 50% methanol that every 1ml is made and contains
The solution of 20~30 μ g to get；
The preparation of test solution：Took this product powder 1g of No. three sieves, it is accurately weighed, set in round-bottomed flask, precision plus
Enter 50% 20~30ml of methanol, weighed weight is heated to reflux 1 hour, lets cool, then weighed weight, and less loss is supplied with 50% methanol
Weight, shake up, filter, take subsequent filtrate to get；
Measuring method：It is accurate respectively to draw reference substance solution and each 5~15 μ l of test solution, liquid chromatograph is injected, is surveyed
It is fixed to get.
In oxalic detection method above-mentioned, the content assaying method of the Saponaretin is：
According to《Chinese Pharmacopoeia》High effective liquid chromatography for measuring；
Chromatographic condition and system suitability：Using octadecylsilane chemically bonded silica as filler；With acetonitrile：0.1%
Phosphoric acid solution=15：85 be mobile phase；Detection wavelength is 338nm；Number of theoretical plate is calculated by Saponaretin peak is not less than 5000；
The preparation of reference substance solution：Take Saponaretin reference substance appropriate, it is accurately weighed, add 50% methanol that every 1ml is made and contains
The solution of 26 μ g to get；
The preparation of test solution：No. three this product powder were taken to sieve 1g, it is accurately weighed, it sets in round-bottomed flask, precision adds
Enter 50% methanol 25ml, weighed weight is heated to reflux 1 hour, lets cool, then weighed weight, and the weight of less loss is supplied with 50% methanol
Amount, shake up, filter, take subsequent filtrate to get；
Measuring method：It is accurate respectively to draw reference substance solution and each 10 μ l of test solution, liquid chromatograph is injected, is measured,
To obtain the final product.
In oxalic detection method above-mentioned, the detection method is：
【Character】This product root is cylinder, slightly distorts, and has branch, surface brown or brownish red, has longitudinal grin, and root head is slightly swollen
Greatly, matter is hard, frangibility, section canescence；Stem, branch are become mildewed by thin；Leaf alternate, palmately compound leaf have handle, stipule and petiole adhesion,
3 pieces of leaflet, heart-shaped, long 5~10cm, stockless；Flower yellow, equal 5 of sepal, petal；Capsule is closely cylindrical, 5, rib, soft
Hair, seed is small, flat oval, brown；Has acid gas, taste is salty and sour and astringent.
【Differentiate】(1) this product powder taupe is to yellowish-brown；Nonglandular hair is a lot of, predominantly unicellular, apex point, wall thickness,
Has verruca；It can be seen that another nonglandular hair, apex blunt circle, wall glimmer are slided；Calcium oxalate prismatic crystal is square in stem parenchyma cell,
3~20 μm of diameter；Fiber pit is apparent, wall thickness, 5~32 μm of diameter；Conduit is that spiral duct, scalariform duct and bordered pit are led
Pipe.
(2) this product powder 0.5g is taken, methanol 10ml is added, is ultrasonically treated 30 minutes, filtration takes filtrate molten as test sample
Liquid；Creeping oxalis control medicinal material 0.5g separately is taken, is made in the same way of control medicinal material solution；According to《Chinese Pharmacopoeia》Thin-layered chromatography is tested, and is inhaled
Each 5 μ l of above two solution are taken, are put respectively on same silica G plate, with chloroform：Methanol：Formic acid=8：1：0.1 is expansion
Agent is unfolded, and takes out, dries, set and inspected under 365nm ultraviolet lamps；In test sample chromatography, in position corresponding with control medicinal material chromatography
It sets, shows the fluorescence spot of same color.
【It checks】
Moisture takes dry creeping oxalis, shines《Chinese Pharmacopoeia》Four general rules of version in 2015,0,832 second method is detected；
Total ash takes dry creeping oxalis, shines《Chinese Pharmacopoeia》Four general rules 2302 of version in 2015 are detected；
Acid-insoluble ash takes dry creeping oxalis, shines《Chinese Pharmacopoeia》Four general rules 2302 of version in 2015 are detected；
【Extract】Dry creeping oxalis is taken, is shone《Chinese Pharmacopoeia》Four general rules of version in 2015,2201 ethanol soluble extractives measuring method
Hot dipping under measures, and uses ethanol as solvent；
【Assay】According to《Chinese Pharmacopoeia》High effective liquid chromatography for measuring；
Chromatographic condition and system suitability, using octadecylsilane chemically bonded silica as filler；With acetonitrile：0.1%
Phosphoric acid solution=15：85 be mobile phase；Detection wavelength is 338nm；Number of theoretical plate is calculated by Saponaretin peak is not less than 5000；
The preparation of reference substance solution：Take Saponaretin reference substance appropriate, it is accurately weighed, add 50% methanol that every 1ml is made and contains
The solution of 26 μ g to get；
The preparation of test solution：Took this product powder 1g of No. three sieves, it is accurately weighed, set in round-bottomed flask, precision plus
Enter 50% methanol 25ml, weighed weight is heated to reflux 1 hour, lets cool, then weighed weight, and the weight of less loss is supplied with 50% methanol
Amount, shake up, filter, take subsequent filtrate to get；
Measuring method：It is accurate respectively to draw reference substance solution and each 10 μ l of test solution, liquid chromatograph is injected, is measured,
To obtain the final product.
Inventor has carried out a large amount of experiment, is the research of detection method of the present invention below：
Experimental example 1：Indentification by TLC
1 instrument and reagent
1.1 instrument
3 thin-layer chromatography imaging systems of CAMAG REPROSTAR (Ka Ma companies of Switzerland)；CQ-250A-ST ultrasonic cleanings
Instrument (Shanghai leap medical optical instrument factory)；XTP-A500 types multifunctional crusher (Yongkang City red sun electromechanics Co., Ltd)；
EL204 electronic balances (plum Teller-support benefit Instrument Ltd.)；The laboratories WP- Μ P-II-20 ultrapure water machine (Sichuan water
That Water Management Equipment Ltd.).
1.2 reagent
Control medicinal material picks up from Guizhou Province, is identified as by Guizhou pharmaceutical college of medical university specimen museum associate professor Long Qingde
Oxalis corniculata L..Ethyl acetate (AR, the upper smooth Science and Technology Ltd. of Haitai)；Methanol, ether, ethyl alcohol, benzene (AR,
Sinopharm Chemical Reagent Co., Ltd.)；Chloroform, acetic acid, dichloromethane (AR, Shanghai Shen Bo Chemical Co., Ltd.s)；First
Acid, hexamethylene (AR, Tianjin Ke Miou reagents Co., Ltd)；Sulfuric acid, hydrochloric acid (AR, Chongqing Chuan Dong chemical industry (group) limited public affairs
Department)；Thin-layer chromatography silica gel plate G (Qingdao Marine Chemical Co., Ltd., Yantai Jiang You silica gel development corporation, Ltd., Qingdao Ding Kang silicon
Glue Co., Ltd).
Creeping oxalis, is identified as totally by University Medical institute of Guizhou medical university specimen museum associate professor Long Qingde by 12 batches
It is shown in Table 1 to the fresh or dry herb of Oxalis corniculata L., number and collection.
1 creeping oxalis medicinal material information of table
2, test method
2.1 proper mass standard Thin Layer discrimination methods
《Guizhou Province's Chinese medicine, Ethnic crude drugs quality standard》Version in 2003 records " creeping oxalis " medicinal material【Differentiate】Differentiate under
(2) it is " to take this product powder 3g, add water 10ml, with hydrochloric acid tune pH value to 2~3, be heated to reflux 3 hours, let cool, filter, filtrate is used
Equivalent ether extracts, and divides and takes ether layer, waves to 1ml, as test solution.Creeping oxalis control medicinal material 3g separately is taken, is made in the same way of pair
According to medicinal material solution.According to thin-layered chromatography (《Chinese Pharmacopoeia》One VI B of annex) experiment, 5 μ l of above-mentioned solution are drawn, are put respectively in same
On one silica gel g thin-layer plate, with benzene-methanol-acetic acid (45：8：4) it is solvent, is unfolded, takes out, dry, be placed in ultraviolet lamp
It is inspected under (365nm).In test sample chromatography, on position corresponding with control medicinal material chromatography, the fluorescence spot of same color is shown；
The lamellae is flung into acetic acid, is sprayed with 0.05% bromophenol blue solution.In test sample chromatography, in position corresponding with control medicinal material chromatography
It sets, shows the blue spot of same color." tested according to this method, the results are shown in Figure 1, and (lot number is respectively
20161001、20161017、20170701)。
2.2 indentification by TLC are revised
2.2.1 chromatographic condition and system suitability (specificity experiment)
This product powder 0.5g is taken, methanol 10ml is added, is ultrasonically treated 30 minutes, filtration takes filtrate as test solution.Separately
Creeping oxalis control medicinal material 0.5g is taken, control medicinal material solution is made in the same way of.According to thin-layered chromatography (《Chinese Pharmacopoeia》Version four in 2015
General rule 0502) experiment, each 5 μ l of above-mentioned solution are drawn, are put respectively on same silica G plate, with chloroform-methyl alcohol-formic acid (8：
1：0.1) it is solvent, is unfolded, takes out, dry, set and inspected under ultraviolet lamp (365nm).
Using 5 batches of creeping oxalis samples of this method pair (lot number is respectively 20161001,20161002,20161017,
20160507,20170529) it is analyzed, the results are shown in Figure 2.In test sample chromatography, corresponding to control medicinal material chromatography
Position on, show the spot of same color, this method prepared compared with primary standard method test solution it is easy, fast, Chromatographic information
It is abundant,
2.2.2 serviceability test
2.2.2.1 different brands thin-layer chromatography silica G plate is investigated
According to above-mentioned TLC Identification, investigated respectively Qingdao Haiyang silica G plate, Qingdao Ding Kang silica Gs plate and
The expansion effect of Yantai river friend's silica gel H SG plates, is as a result shown in Fig. 3.
According to the silica G plate of three brands it is found that the separating degree of Qingdao Haiyang and Qingdao Ding Kang silica G plates is almost the same,
Illustrate that its durability is preferable, Yantai river friend's Huanghai Sea silica gel H SG plates are efficient plates, the more other two kinds of ordinary silicons of the spot separated
Glue G plates are more, from the economic and practical common silica G plate of angle Selection.
2.2.2.2 the investigation of difference expansion humidity
The expansion envionmental humidity adjusted respectively with various concentration sulfuric acid is 32%, 58%, 72%, at a temperature of 25 DEG C
The effect of different relative humidity expansion is investigated respectively.
Shown in Fig. 4 results, though the band of chromatogram is clear under different humidity, Rf value differents, however remain to compared with
Differentiate medicinal material well, illustrates that the humidity durability is preferable.
2.2.2.3 the investigation of difference expansion temperature
Respectively at 10 DEG C, 25 DEG C, 35 DEG C, relative humidity is 58% time expansion, investigates influence of the different temperatures to expansion, such as
Shown in Fig. 5.
Shown in Fig. 5 results, the band of chromatogram is clear under different temperatures, the different unobvious of Rf value differences, illustrate the medicinal material by
The influence of temperature is little.
2.2.2.4 test solution study on the stability
By with a batch of this product powder before 3 days, before 2 days, before 1 day, that the same day by above-mentioned method prepares test sample is molten
Liquid is put respectively on same silica G plate, is unfolded, colour developing, as shown in Figure 6.
The results show that the chromatogram after the test solution placed 1~3 day is unfolded is almost the same, show test solution
It had good stability at 3 days.
3. sample measures
According to above-mentioned TLC Identification, 12 batches of samples are measured, shown in result figure 7.
The results show that each batch of sample meets regulation.
Experimental example 2：Determination of moisture
According to《Chinese Pharmacopoeia》0832 aquametry of version general rule (the second method oven drying method) measurement in 2015, takes this product powder
(crossing No. two sieves) 2g, it is accurately weighed, it is laid in the flat measuring cup of dry constant weight, thickness is no more than 5mm, accurately weighed, opens
It is bottle cap opened 5 hours dry at 105 DEG C, bottle cap is covered, in dislocation drier, is let cool 30 minutes, it is accurately weighed, then in above-mentioned temperature
Degree is 1 hour dry, lets cool, weighs, and until the difference weighed twice in succession is no more than 5mg, according to less loss weight, calculates for examination
Water content (%) in product, the results are shown in Table 2.
2 oxalic determination of moisture result of table
From 2 result of table as it can be seen that 12 batches of creeping oxalis moisture content ranges are 6.66%~12.1%.
Experimental example 3：Total ash content measures
According to《Chinese Pharmacopoeia》2302 Ash determination method of version general rule measures within 2015, takes this product powder 3g, sets ignition to constant weight
Crucible in, weighed weight (accurate 0.01g) is slowly blazing, pays attention to avoiding burning, until completely charing when, gradually rise temperature
To 550 DEG C, makes to be ashed completely and calculate the content (%) of total ash in test sample according to residue weight to constant weight, the results are shown in Table
3。
3 oxalic total ash measurement result of table
From table 3 the results show that total ash 9.16%~13.73% in 12 batches of creeping oxalis medicinal materials.
Experimental example 4：Acid-insoluble ash measures
The ash content obtained by item is taken, dilute hydrochloric acid 10ml is carefully added into crucible, crucible is covered with surface plate, sets in water-bath
Heating 10 minutes, surface plate are rinsed with hot water 5ml, and washing lotion is incorporated in crucible, is filtered with ashless filter paper, the residue water in crucible
It washes on filter paper, and washs until the not aobvious chloride reaction of washing lotion.For filter residue together in the same crucible of filter paper dislocation, drying is vehement
It burns to constant weight.According to residue weight, the content (%) of acid-insoluble ash in test sample is calculated, the results are shown in Table 4.The results show that
Acid-insoluble ash 1.58%~4.63% in 12 batches of creeping oxalis medicinal materials.
4 oxalic total ash measurement result of table
Experimental example 5：Extract content measures
The main chemical compositions dissolubility and use habit contained according to creeping oxalis, its ethanol soluble extractives of Selecting research.According to
《Chinese Pharmacopoeia》Ethanol soluble extractives measuring method hot dipping in four 2201 Extract mensurations of general rule of version in 2015, using ethyl alcohol
Determination of extractives is carried out for solvent；
This product powder (cross No. two sieve) 2g is taken, it is accurately weighed, it sets in the conical flask of 100ml, precision plus ethyl alcohol 50ml are close
Plug, weighed weight after standing 1 hour, connect reflux condensing tube, are heated to boiling, and keep slightly boiling 1 hour, after letting cool, remove
Conical flask, close plug, then weighed weight are supplied less loss weight with ethyl alcohol, are shaken up, and are filtered with dry filter, precision measures filtrate
25ml, which is set, have been dried into the evaporating dish of constant weight, 3 hours dry in 105 DEG C after being evaporated in water-bath, is set cooling 30 in drier
Minute, rapid accurately weighed weight calculates the content (%) of ethanol soluble extractives in test sample with dry product.As a result such as 5 institute of table
Show.
5 oxalic ethanol soluble extractives of table survey result
According to 12 batch creeping oxalis ethanol soluble extractives 5.22%~15.8%.
Experimental example 5：The assay of Saponaretin
Inventor has found that, for creeping oxalis, having more document report creeping oxalis content has more Huang in the course of the research
Ketone and phenolic acid compound, report compound that it contains have Vitexin, isovitexin, robinin, robinin, tartaric acid,
Vanillic acid, Luteolin, hydroxycinnamic acid, caffeic acid, Quercetin and gallic acid etc. are used by fingerprint map analyzing technology
Ultraviolet and mass detector etc., the reference substance bought using National Institute for Food and Drugs Control, to caffeic acid, Quercetin, wood
The index components such as sweet-scented osmanthus grass element, gallic acid, orientin carry out multiple batches of fingerprint map analyzing, and analysis result shows these chemical combination
Object content is too low, or differs greatly in each batch medicinal material, therefore is not suitable for as quality control index, by oxalic master
Chemical composition analysis is wanted to study, discovery Saponaretin is its main representative flavone compound, therefore Saponaretin is selected to make
For creeping oxalis assay control index components.
The characteristics of according to this product, with reference to (《Chinese Pharmacopoeia》9101 drug standard analysis method of version general rule is tested within 2015
Demonstrate,prove guideline) and《It Guizhou Province's Chinese medicine, Ethnic crude drugs quality standard and drafts and illustrates Compiling Technique requirement》Related content, system
The content that HPLC methods measure creeping oxalis medicinal material Saponaretin is determined.
1 instrument and reagent
1.1 instrument
3000 type high performance liquid chromatographs of UlMate (Thermo Fisher, including system controller, infusion pump, degassing
Component, low pressure gradient component, autosampler, column oven, temperature control sample room, Μ V-VIS detectors and Chromeleon chromatographies
Data workstation)；EL204 types electronic balance (plum Teller-support benefit instrument Shanghai Co., Ltd)；The desk-top freezings of Allegra64R
Centrifuge (U.S.'s Beckman)；WP- Μ P-IV-20 types ultrapure water machines (Sichuan Water Technology Development Co., Ltd.).
1.2 reagent
Saponaretin (Chengdu Zhi Biaohuachun Bioisystech Co., Ltd, purity 98.47%, lot number：170904)；Acetonitrile
(GR, Sinopharm Chemical Reagent Co., Ltd., lot number：20170619)；Methanol (AR, Sinopharm Chemical Reagent Co., Ltd.,
Lot number：20170925)；Phosphoric acid；Water is ultra-pure water.
Creeping oxalis medicinal material information is the same as table 1.
2 chromatographic conditions
Chromatographic column is Venusil XBP C18 (L) (4.6mm × 250mm, 5 μm)；- 0.1% phosphoric acid solution (15 of acetonitrile：
85) it is mobile phase, flow velocity 1ml/min, 35 DEG C of chromatogram column temperature, Detection wavelength 338nm；10 μ l of sample size, number of theoretical plate
5000 should be not less than by being calculated with Saponaretin peak.
It is prepared by 3 test solutions
3.1 extracting methods are investigated
Same batch creeping oxalis medicinal material (20160924) is taken, is ultrasonically treated respectively, three kinds of Soxhlet and refluxing extraction carry
The investigation of method is taken, is extracted 1 hour respectively, the results are shown in Table 6, the results showed that Saponaretin recovery rate when using refluxing extraction
Highest, it is thus determined that refluxing extraction is extracting method.
6 extracting method of table investigates result
3.2 Extraction solvents are investigated
Same batch creeping oxalis medicinal material (20160924) is taken, respectively to the methanol of different volumes score, 75% methanol, 50%
Methanol, 25% methanol and 95% ethyl alcohol, 75% ethyl alcohol, 50% ethyl alcohol, 25% ethyl alcohol extract solvent investigation, and reflux respectively carries
Take 1 hour, the results are shown in Table 7, the results showed that 50% methanol to Saponaretin recovery rate highest, therefore select 50% methanol as
Extraction solvent.
7 Extraction solvent of table investigates result
3.3 extraction times were investigated
Same batch creeping oxalis medicinal material (20160924) is taken, using 50% methanol as Extraction solvent, is extracted using reflux side
Method extract respectively 0.5 hour, 1 hour, 2 hours, 4 hours to investigate extraction time, the results showed that extraction time is 1 hour, different
Vitexina has extracted completely, and when continuing growing the time, recovery rate is not further added by, it is thus determined that extraction time is 1 hour.
8 extraction time of table investigates result
By investigating optimization above, test solution preparation method is：Took the creeping oxalis medicinal powder 1g of No. three sieves, essence
It is close weighed, it sets in round-bottomed flask, 50% methanol 25ml is added in precision, and weighed weight is heated to reflux 1 hour, lets cool, then weighed heavy
Amount, the weight of less loss is supplied with 50% methanol, shakes up, filter, take subsequent filtrate to get.
It is prepared by 4 reference substance solutions
Take Saponaretin reference substance appropriate, it is accurately weighed, add 50% methanol to dissolve, every 1ml is made and contains Saponaretin
The solution of 0.5219mg shakes up to get reference substance storing solution.Precision measurement reference substance solution storing solution is appropriate, is configured to concentration
For 26.10 μ g/ml reference substance solutions.
5 methodology validations
5.1 specificities are tested
Each 10 μ l of reference substance solution, test solution are drawn respectively injects liquid chromatograph, record chromatography (Fig. 8).From figure
In as it can be seen that Saponaretin retention time be 14.0 minutes, the separation of Saponaretin and other components peak under this experimental condition
Degree is more than 1.5, and the chromatographic peak ultraviolet spectrogram consistent with retention time in reference substance chromatography is consistent (Fig. 9) in test sample chromatography,
Illustrate that this method specificity is good.Number of theoretical plate is calculated as 6000 with Saponaretin peak, therefore provides number of theoretical plate with Saponaretin
It calculates, 5000 should be not less than.
5.2 linear relationships are tested
Accurate amount reference substance storing solution takes in right amount respectively, is placed in 10ml volumetric flasks, with 50% methanol dilution to scale, shakes
It is even, with a concentration of 5.20,10.4,26.1,52.2,78.3 μ g/ml control series product solution, be injected separately into liquid chromatogram
Instrument records chromatographic peak area, and with reference substance concentration (μ g/ml) for abscissa (X), peak area is that ordinate (Y) drawing is bent
Line carries out recurrence processing, the results showed that reference substance concentration is in good linear relationship, regression equation with peak area：Y=
573.18X-0.0319 r=0.9990, the range of linearity：5.20~78.3 μ g/ml, linearity curve such as Figure 10.
9 range of linearity of table
5.3 precision test
5.3.1 repetitive test
Each 3 parts of creeping oxalis medicinal material (20160924) powder 0.5g, 1g, 1.5g is taken respectively, it is accurately weighed, by test solution
Preparation method prepares 9 parts of test solution；Reference substance solution is prepared by reference substance solution preparation method.Sample introduction reference substance is molten respectively
Liquid and test solution measure and calculation, the results are shown in Table 10, show that this method repeatability is good.
10 repetitive test table of table
5.3.2 Intermediate precision is tested
With different experiment people, creeping oxalis medicinal material (20160924) powder 1g 3 is taken respectively as stated above in different time
Part, it is accurately weighed, respectively test solution is prepared by test solution preparation method；By the preparation pair of reference substance solution preparation method
According to product solution, difference sample introduction reference substance solution and each test solution.11 are the results are shown in Table, not same date, different analysis personnel inspections
It surveys the result shows that the Intermediate precision of method is good.
11 Intermediate precision of table tests table
5.4 recovery test
Creeping oxalis medicinal material (20160924) powder 0.5g of 6 parts of known contents is taken, it is accurately weighed, it is measured by sample is weighed
Saponaretin reference substance is added in the background values of ingredient, and test solution is prepared by test solution preparation method；It is molten by reference substance
Liquid and preparation method thereof prepares reference substance solution, respectively sample introduction reference substance solution and test solution.12 are the results are shown in Table, shows this method
Accuracy is good.
12 recovery test result of table
5.5 serviceability test
5.5.1 test solution stability test
Test solution is prepared by test solution preparation method, in 0,1,2,4,8,24 hour difference sample introduction, 5 records
Chromatogram investigates test solution stability, and result of calculation is shown in Table 13, shows that test solution is stablized in 24 hours.
13 stability test of table is investigated
5.5.2 different mobile phase ratios
By test solution preparation method 3 parts of test solutions of parallel preparation, by the preparation pair of reference substance solution preparation method
Only change mobile phase ratio, i.e., respectively with -0.1% phosphoric acid solution (14 of acetonitrile by chromatographic condition is drafted according to product solution：86), second
- 0.1% phosphoric acid solution (15 of nitrile：And -0.1% phosphoric acid solution (16 of acetonitrile 85)：84) it is mobile phase, sample introduction reference substance solution and confession
Test sample solution records chromatogram, calculates content, the results are shown in Table 14.
The different mobile phase ratio measurement results of table 14 compare
5.5.3 different pH value are investigated
By test solution preparation method 3 parts of test solutions of parallel preparation, by the preparation pair of reference substance solution preparation method
Only change aqueous phase acidity, i.e., respectively with -0.05% phosphoric acid solution (15 of acetonitrile by chromatographic condition is drafted according to product solution：85), second
- 0.1% phosphoric acid solution (15 of nitrile：And -0.15% phosphoric acid solution (15 of acetonitrile 85)：85) be mobile phase, sample introduction reference substance solution and
Test solution records chromatogram, calculates content, the results are shown in Table 15.
The different pH value measurement results of table 15 compare
5.5.4 investigation different in flow rate
By test solution preparation method 3 parts of test solutions of parallel preparation, by the preparation pair of reference substance solution preparation method
Only change flow velocity by chromatographic condition is drafted according to product solution, i.e., respectively using 0.9,1.0 and 1.1ml/min as flow velocity, sample introduction control
Product solution and test solution record chromatogram, calculate content, the results are shown in Table 16.
16 measurement result different in flow rate of table compares
5.5.5 different chromatographic columns compare
By test solution preparation method 3 parts of test solutions of parallel preparation, by the preparation pair of reference substance solution preparation method
According to product solution, by chromatographic condition is drafted, with different chromatographic columns, sample introduction reference substance solution and test solution record chromatogram, meter
Content is calculated, the results are shown in Table 17.
The different chromatographic column measurement results of table 17 compare
5.5.6 different Detection wavelengths
By test solution preparation method 3 parts of test solutions of parallel preparation, by the preparation pair of reference substance solution preparation method
, with same branch chromatographic column, only change Detection wavelength, i.e., respectively with 335,338 and 340nm by chromatographic condition is drafted according to product solution
For wavelength, sample introduction reference substance solution and test solution record chromatogram, calculate content, the results are shown in Table 18.
The different Detection wavelength measurement results of table 18 compare
5.5.7 different chromatogram column temperatures
By test solution preparation method 3 parts of test solutions of parallel preparation, by the preparation pair of reference substance solution preparation method
Only change chromatogram column temperature, i.e., respectively with 32,35 and 38 DEG C for column temperature, sample introduction reference substance by chromatographic condition is drafted according to product solution
Solution and test solution record chromatogram, calculate content, the results are shown in Table 19.
The different chromatogram column temperature measurement results of table 19 compare
5.5.8 different model instrument
By test solution preparation method 3 parts of test solutions of parallel preparation, by the preparation pair of reference substance solution preparation method
According to product solution, by chromatographic condition is drafted, with same branch chromatographic column, in different liquid chromatographs, i.e., respectively with UlMate 3000
(double ternarys), UlMate3000 and Shimadzu Prominence LC-20A sample introductions reference substance solutions and test solution record chromatography
Figure calculates content, the results are shown in Table 20.
20 different manufacturers of table and model HPLC measurement results compare
6 samples measure
Each two parts of each batch creeping oxalis medicinal powder 1g is taken, it is accurately weighed, it is prepared for examination by test solution preparation method
Product solution prepares reference substance solution by reference substance solution preparation method, and sample introduction is analyzed under conditions of drafting, and records chromatogram,
Content is calculated, the results are shown in Table 21.The result shows that 12 batches of creeping oxalis medicinal material Saponaretin contents are between 0.036%~0.14%.
21 creeping oxalis medicinal material assay result of table
The beneficial effects of the present invention are：A kind of oxalic detection method is provided；Using indentification by TLC experiment pair
Creeping oxalis is differentiated, is measured to creeping oxalis moisture, total ash, acid-insoluble ash, extract, and to Saponaretin
Content is measured, and the detection method is accurate, and high sensitivity is reproducible, as a result reliably, can effectively control oxalic matter
Amount, it is ensured that oxalic drug effect.
Description of the drawings
Fig. 1 is primary standard method TLC chromatograms；1~3 is 3 batches of samples；4 be control medicinal material；
Fig. 2 is creeping oxalis indentification by TLC system suitability figure；1~5 is 5 batches of samples；6 be control medicinal material；
Fig. 3 is different brands thin-layer chromatography silica G plate expansion TLC figures；1~3 is 3 batches of samples；4 be control medicinal material；
Fig. 4 is different expansion humidity TLC figures；1~3 is 3 batches of samples；4 be control medicinal material；
Fig. 5 is different expansion temperature TLC figures；1~3 is 3 batches of samples；4 be control medicinal material
Fig. 6 is test solution study on the stability TLC figures；1 is the same day；2 be placement 1 day；3 be placement 2 days；4 be placement 3
It；5 be control medicinal material；
Fig. 7 is the TLC figures of 12 batches of samples；1~12 is 12 batches of samples；13 be control medicinal material；
Fig. 8 is reference substance and test solution chromatogram；
Fig. 9 is reference substance and test solution spectrogram；
Figure 10 is linearity curve；
Figure 11 is creeping oxalis medicinal material microscopical characters figure；1- nonglandular hairs, 2- stomatas, 3- pollen grains, 4- conduits, the calcium oxalate sides 5-
Crystalline substance, 6- epidermal cells, 7- kind chrotoplasts, 8- fibers.
With reference to embodiment, the present invention is further illustrated
Specific implementation mode
Embodiment：
A kind of oxalic detection method,
【Character】This product root is cylinder, slightly distorts, and has branch, surface brown or brownish red, has longitudinal grin, and root head is slightly swollen
Greatly, matter is hard, frangibility, section canescence；Stem, branch are become mildewed by thin；Leaf alternate, palmately compound leaf have handle, stipule and petiole adhesion,
3 pieces of leaflet, heart-shaped, long 5~10cm, stockless；Flower yellow, equal 5 of sepal, petal；Capsule is closely cylindrical, 5, rib, soft
Hair, seed is small, flat oval, brown；Has acid gas, taste is salty and sour and astringent.
【Differentiate】(1) this product powder taupe is to yellowish-brown；Nonglandular hair is a lot of, predominantly unicellular, apex point, wall thickness,
Has verruca；It can be seen that another nonglandular hair, apex blunt circle, wall glimmer are slided；Calcium oxalate prismatic crystal is square in stem parenchyma cell,
3~20 μm of diameter；Fiber pit is apparent, wall thickness, 5~32 μm of diameter；Conduit is that spiral duct, scalariform duct and bordered pit are led
Pipe.
(2) this product powder 0.5g is taken, methanol 10ml is added, is ultrasonically treated 30 minutes, filtration takes filtrate molten as test sample
Liquid；Creeping oxalis control medicinal material 0.5g separately is taken, is made in the same way of control medicinal material solution；According to《Chinese Pharmacopoeia》Thin-layered chromatography is tested, and is inhaled
Each 5 μ l of above two solution are taken, are put respectively on same silica G plate, with chloroform：Methanol：Formic acid=8：1：0.1 is expansion
Agent is unfolded, and takes out, dries, set and inspected under 365nm ultraviolet lamps；In test sample chromatography, in position corresponding with control medicinal material chromatography
It sets, shows the fluorescence spot of same color.
【It checks】
Moisture takes dry creeping oxalis, shines《Chinese Pharmacopoeia》Four general rules of version in 2015,0,832 second method is detected；
Total ash takes dry creeping oxalis, shines《Chinese Pharmacopoeia》Four general rules 2302 of version in 2015 are detected；
Acid-insoluble ash takes dry creeping oxalis, shines《Chinese Pharmacopoeia》Four general rules 2302 of version in 2015 are detected；
【Extract】Dry creeping oxalis is taken, is shone《Chinese Pharmacopoeia》Four general rules of version in 2015,2201 ethanol soluble extractives measuring method
Hot dipping under measures, and uses ethanol as solvent；
【Assay】According to《Chinese Pharmacopoeia》High effective liquid chromatography for measuring；
Chromatographic condition and system suitability, using octadecylsilane chemically bonded silica as filler；With acetonitrile：0.1%
Phosphoric acid solution=15：85 be mobile phase；Detection wavelength is 338nm；Number of theoretical plate is calculated by Saponaretin peak is not less than 5000；
The preparation of reference substance solution：Take Saponaretin reference substance appropriate, it is accurately weighed, add 50% methanol that every 1ml is made and contains
The solution of 26 μ g to get；
The preparation of test solution：Took this product powder 1g of No. three sieves, it is accurately weighed, set in round-bottomed flask, precision plus
Enter 50% methanol 25ml, weighed weight is heated to reflux 1 hour, lets cool, then weighed weight, and the weight of less loss is supplied with 50% methanol
Amount, shake up, filter, take subsequent filtrate to get；
Measuring method：It is accurate respectively to draw reference substance solution and each 10 μ l of test solution, liquid chromatograph is injected, is measured,
To obtain the final product.
Claims (6)
1. a kind of oxalic detection method, it is characterised in that：Content assaying method including discrimination method and Saponaretin.
2. oxalic detection method according to claim 1, it is characterised in that：The discrimination method is：Take this product powder
0.1 ~ 1g of end adds 5 ~ 15ml of methanol, is ultrasonically treated 10 ~ 50 minutes, and filtration takes filtrate as test solution；Separately take creeping oxalis
Control medicinal material 0.5g adds 5 ~ 15ml of methanol, is ultrasonically treated 10 ~ 50 minutes, and filtration takes filtrate medicinal material solution as a contrast；According to《In
State's pharmacopeia》Thin-layered chromatography is tested, and each 1 ~ 8 μ l of above two solution are drawn, and is put respectively on same silica G plate, with three chloromethanes
Alkane：Methanol：Formic acid=5 ~ 10：0.5~1.5：0.05 ~ 0.15 is solvent, is unfolded, takes out, dry, set 360 ~ 370nm ultraviolet lights
It is inspected under lamp；In test sample chromatography, on position corresponding with control medicinal material chromatography, the fluorescence spot of same color is shown.
3. oxalic detection method according to claim 2, it is characterised in that：The discrimination method is：Take this product powder
Last 0.5g adds methanol 10ml, is ultrasonically treated 30 minutes, and filtration takes filtrate as test solution；Separately take creeping oxalis control medicinal material
0.5g adds methanol 10ml, is ultrasonically treated 30 minutes, and filtration takes filtrate medicinal material solution as a contrast；According to《Chinese Pharmacopoeia》Thin layer color
Spectrometry is tested, and each 5 μ l of above two solution are drawn, and is put respectively on same silica G plate, with chloroform-methyl alcohol-formic acid=8：
1：0.1 is solvent, is unfolded, and takes out, dries, set and inspected under 365nm ultraviolet lamps；In test sample chromatography, with control medicinal material
On the corresponding position of chromatography, the fluorescence spot of same color is shown.
4. oxalic detection method according to claim 1, it is characterised in that：The assay side of the Saponaretin
Method is：
According to《Chinese Pharmacopoeia》High effective liquid chromatography for measuring;
Chromatographic condition and system suitability：Using octadecylsilane chemically bonded silica as filler；With acetonitrile：0.1% phosphoric acid is molten
Liquid=10 ~ 20：90 ~ 80 be mobile phase；Detection wavelength is 330 ~ 340 nm；Number of theoretical plate is not less than by the calculating of Saponaretin peak
5000；
The preparation of reference substance solution：Take Saponaretin reference substance appropriate, it is accurately weighed, add 50% methanol that every 1 ml is made and contains 20 ~ 30
The solution of μ g to get；
The preparation of test solution：This product powder 1 g of No. three sieves was taken, it is accurately weighed, it sets in round-bottomed flask, precision is added
50% methanol, 20 ~ 30 ml, weighed weight are heated to reflux 1 hour, let cool, then weighed weight, and the weight of less loss is supplied with 50% methanol
Amount, shake up, filter, take subsequent filtrate to get；
Measuring method：It is accurate respectively to draw reference substance solution and each 5 ~ 15 μ l of test solution, liquid chromatograph is injected, is measured, i.e.,
.
5. oxalic detection method according to claim 4, it is characterised in that：The assay side of the Saponaretin
Method is：
According to《Chinese Pharmacopoeia》High effective liquid chromatography for measuring；
Chromatographic condition and system suitability：Using octadecylsilane chemically bonded silica as filler；With acetonitrile：0.1% phosphoric acid is molten
Liquid=15：85 be mobile phase；Detection wavelength is 338 nm；Number of theoretical plate is calculated by Saponaretin peak is not less than 5000；
The preparation of reference substance solution：Take Saponaretin reference substance appropriate, it is accurately weighed, add 50% methanol that every 1 ml is made and contains 26 μ g
Solution to get；
The preparation of test solution：This product powder 1 g of No. three sieves was taken, it is accurately weighed, it sets in round-bottomed flask, precision is added
50% methanol, 25 ml, weighed weight are heated to reflux 1 hour, let cool, then weighed weight, and the weight of less loss is supplied with 50% methanol,
Shake up, filter, take subsequent filtrate to get；
Measuring method：It is accurate respectively to draw reference substance solution and each 10 μ l of test solution, inject liquid chromatograph, measure to get.
6. oxalic detection method according to claim 1, it is characterised in that：The detection method is：
【Character】This product root is cylinder, slightly distorts, and has branch, surface brown or brownish red, has longitudinal grin, and root head is slightly expanded,
Matter is hard, frangibility, section canescence；Stem, branch are become mildewed by thin；Leaf alternate, palmately compound leaf have handle, stipule and petiole adhesion, leaflet
It is 3 pieces, heart-shaped, long 5~10cm, stockless；Flower yellow, equal 5 of sepal, petal；Capsule is closely cylindrical, 5, rib, by pubescence,
Seed is small, flat oval, brown；Has acid gas, taste is salty and sour and astringent；
【Differentiate】（1）This product powder taupe is to yellowish-brown；Nonglandular hair is a lot of, predominantly unicellular, and apex point, wall thickness has wart
Shape protrusion；It can be seen that another nonglandular hair, apex blunt circle, wall glimmer are slided；Calcium oxalate prismatic crystal is square in stem parenchyma cell, diameter 3
~20μm；Fiber pit is apparent, wall thickness, 5 ~ 32 μm of diameter；Conduit is spiral duct, scalariform duct and bordered pit vessel；
（2）This product powder 0.5g is taken, methanol 10ml is added, is ultrasonically treated 30 minutes, filtration takes filtrate as test solution；Separately
Creeping oxalis control medicinal material 0.5g is taken, control medicinal material solution is made in the same way of；According to《Chinese Pharmacopoeia》Thin-layered chromatography is tested, and is drawn above-mentioned
Each 5 μ l of two kinds of solution are put respectively on same silica G plate, with chloroform：Methanol：Formic acid=8：1：0.1 is solvent, exhibition
It opens, takes out, dry, set and inspected under 365nm ultraviolet lamps；In test sample chromatography, on position corresponding with control medicinal material chromatography,
The fluorescence spot of aobvious same color；
【It checks】
Moisture takes dry creeping oxalis, shines《Chinese Pharmacopoeia》Four general rules of version in 2015,0,832 second method is detected；
Total ash takes dry creeping oxalis, shines《Chinese Pharmacopoeia》Four general rules 2302 of version in 2015 are detected；
Acid-insoluble ash takes dry creeping oxalis, shines《Chinese Pharmacopoeia》Four general rules 2302 of version in 2015 are detected；
【Extract】Dry creeping oxalis is taken, is shone《Chinese Pharmacopoeia》Under four general rules of version in 2015,2201 ethanol soluble extractives measuring method item
Hot dipping measure, use ethanol as solvent；
【Assay】According to《Chinese Pharmacopoeia》High effective liquid chromatography for measuring；
Chromatographic condition and system suitability, using octadecylsilane chemically bonded silica as filler；With acetonitrile：0.1% phosphoric acid is molten
Liquid=15：85 be mobile phase；Detection wavelength is 338 nm；Number of theoretical plate is calculated by Saponaretin peak is not less than 5000；
The preparation of reference substance solution：Take Saponaretin reference substance appropriate, it is accurately weighed, add 50% methanol that every 1 ml is made and contains 26 μ g
Solution to get；
The preparation of test solution：Take this product powder（Cross No. three sieves）1 g, it is accurately weighed, it sets in round-bottomed flask, precision is added
50% methanol, 25 ml, weighed weight are heated to reflux 1 hour, let cool, then weighed weight, and the weight of less loss is supplied with 50% methanol,
Shake up, filter, take subsequent filtrate to get；
Measuring method：It is accurate respectively to draw reference substance solution and each 10 μ l of test solution, inject liquid chromatograph, measure to get.
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Application publication date: 20180807 |