CN109946397A - A kind of pithecellobium clypearia method of inspection - Google Patents
A kind of pithecellobium clypearia method of inspection Download PDFInfo
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- CN109946397A CN109946397A CN201910231579.5A CN201910231579A CN109946397A CN 109946397 A CN109946397 A CN 109946397A CN 201910231579 A CN201910231579 A CN 201910231579A CN 109946397 A CN109946397 A CN 109946397A
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- Prior art keywords
- mobile phase
- quercitin
- gallic acid
- reference substance
- pithecellobium clypearia
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Abstract
The invention discloses a kind of pithecellobium clypearia methods of inspection, are related to pithecellobium clypearia inspection technology field, comprising the following steps: S1, carry out gradient elution；S2, preparation reference substance solution；The system of S3, test solution；S4, it is measured；It is accurate respectively to draw reference substance solution and each 10 μ l of test solution, inject liquid chromatograph, measurement, to obtain the final product, the content Con trolling index of the increased gallic acid of the present invention, quercitin, using the quality of digitized norm controlling pithecellobium clypearia, the quality stability of medicinal material can be improved, guarantee the stable and controllable for quality of product.
Description
Technical field
The present invention relates to pithecellobium clypearia inspection technology field, specifically a kind of pithecellobium clypearia method of inspection.
Background technique
Pithecellobium clypearia is Dicotyledoneae, this perennial tall plant of pulse family, and in July, 1984 is by south China Institute of Zoology point
It is Mimosaceae that class room, which identifies former plant, after pulse family, pithecellobium clypearia category be grouped by International Health Organization.Pithecellobium clypearia nature and flavor are bitter
Cold, it is the unique southern medicinal material of a variety of heat toxin diseases for the treatment of that effect is clearing heat and detoxicating, hygroscopic sore.
For pithecellobium clypearia in the method for inspection, conventional method is as follows:
Pithecellobium clypearia character: the pinnate compound leaf with sprig, the tender sprig of children have an apparent vertical rib, and surface brown is to brown
Color, by short fine hair, leaf alternate, slightly shrinkage is in two times pinnate compound leaves after flattening.The nearly diamond shape of vanelets, long 1.3~8.5cm are wide
7~32mm, apex is tapering or anxious sharp, the nearly section shape of base portion, deflection, upper surface sepia, lower surface taupe, Bao Gezhi, easily
It falls off.Gas is micro-, and mildly bitter flavor is puckery.
Microscopical characters: this product cross section: epicuticle cell 1 arranges, and class is rectangular or slightly tangentially extends, and nonglandular hair is more elongated, wall
Has verruca, it is in mastoid process that following table chrotoplast cutin shape thickens more, and nonglandular hair is slightly more, and palisade cell 1 arranges, sponge group
The cell arrangement knitted is loose, and tough shape outside master pulse vascular bundle has bundle-sheath fibrous layer outside.There is collenchymatous cell on the inside of master pulse lower epidermis.
Leaf surface is seen: the wavy bending of upper and lower epidermal cell anticline.Nonglandular hair is unicellular or 2~3 cells composition, wall have
Verruca.Lower epidermis stomata is numerous, flat shaft type.Calcium oxalate prismatic crystal is numerous, is present in fibre bundle peripheral cell, is formed brilliant fine
Dimension.
Thin-layer chromatography: taking this product 5g, grinds, adds water 50ml, boil 30 minutes, filters, and filtrate is concentrated into paste, adds nothing
Water-ethanol 25ml sets and is heated to reflux in water-bath 10 minutes, adds active carbon about 0.3g, stirs, and filtration, filtrate is concentrated into 2ml, as
Test solution separately takes gallic acid reference substance, adds dehydrated alcohol that the solution in every 1ml containing 8mg is made, molten as reference substance
Liquid.It is tested according to thin-layered chromatography [" Chinese Pharmacopoeia " version general rule 0502 in 2015], draws each 2ul of above two solution, respectively point
In on same silica gel g thin-layer plate, with chloroform-acetic ether-methanoic acid (4:1:1) for solvent, it is unfolded, takes out, dry, spray
With 2% ferric trichloride ethanol solution, in sample chromatogram, at the position corresponding to the chromatogram of the reference substance, the spot of same color is shown
Point.
But the method for inspection can not improve the quality of pithecellobium clypearia, therefore propose a kind of new pithecellobium clypearia method of inspection
To solve the above problems.
Summary of the invention
It is mentioned above in the background art to solve the purpose of the present invention is to provide a kind of pithecellobium clypearia method of inspection
Problem.
To achieve the above object, the invention provides the following technical scheme:
A kind of pithecellobium clypearia method of inspection, comprising the following steps:
S1, gradient elution is carried out；
Using octadecylsilane chemically bonded silica as filler；It is flowing with 0.2% phosphoric acid solution using acetonitrile as mobile phase A
Phase B weighs gallic acid, quercitin, and gallic acid Detection wavelength is 270nm, and quercitin Detection wavelength is 350nm.Theoretical plate
Number is calculated by gallic acid peak should be not less than 4000, and 10000 should be not less than by calculating by quercitin peak；Gradient is carried out by following provisions
Elution:
Time is 0-15min, mobile phase A 5%-25%, Mobile phase B 95%-75%；
Time is 15-25min, mobile phase A 25%, Mobile phase B 57%；
Time is 25-27min, mobile phase A 25%-30%, Mobile phase B 75%-70%；
Time is 27-40min, mobile phase A 30%, Mobile phase B 70%.
S2, preparation reference substance solution；
Precision weighs quercitin reference substance 4-10mg, and gallic acid reference substance 4-10mg adds methanol that every 0.8-1.2ml is made
Each gallic acid 0.2-0.4mg, quercitin 10-20 μ g mixed solution to get.
The system of S3, test solution；
This product powder 1.9-2.1g is taken, accurately weighed, water 50mL, weighed weight is added in precision, and close plug gently shakes up, and soaks
It stain 25-35 minutes, is heated to reflux 1 hour, takes out, be cooled to room temperature, then weighed weight, the weight of less loss, then essence are supplied with water
Close addition methanol 48-52ml, weighed weight, close plug gently shake up, and are ultrasonically treated 1 hour, take out, are cooled to room temperature, then weighed
Weight is supplied the weight of less loss with methanol, is shaken up, and filters or is centrifuged, as test solution.
S4, it is measured；
It is accurate respectively to draw reference substance solution and each 10 μ l of test solution, inject liquid chromatograph, measurement to get.
Compared with prior art, the beneficial effects of the present invention are: comparing primary standard detection method, new detection method is increased
The content Con trolling index of gallic acid, quercitin can be improved medicinal material using the quality of digitized norm controlling pithecellobium clypearia
Quality stability guarantees the stable and controllable for quality of product.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
Embodiment 1
A kind of pithecellobium clypearia method of inspection, comprising the following steps:
S1, gradient elution is carried out；
Using octadecylsilane chemically bonded silica as filler；It is flowing with 0.2% phosphoric acid solution using acetonitrile as mobile phase A
Phase B, the regulation according to the form below carry out gradient elution；Gallic acid, quercitin are weighed, gallic acid Detection wavelength is 270nm, Mongolian oak
Skin glycosides Detection wavelength is 350nm.Number of theoretical plate is calculated by gallic acid peak should be not less than 4000, should not be low by the calculating of quercitin peak
In 10000.
| Time (minute) | Mobile phase A (%) | Mobile phase B (%) |
| 0-15 | 5-25 | 95-75 |
| 15-25 | 25 | 75 |
| 25-27 | 25-30 | 75-70 |
| 27-40 | 30 | 70 |
S2, preparation reference substance solution；
Precision weighs quercitin reference substance 4mg, gallic acid reference substance 4mg, adds methanol that each gallic acid of every 0.8ml is made
0.2-0.4mg, 10 μ g of quercitin mixed solution to get.
The system of S3, test solution；
This product powder 1.9g is taken, accurately weighed, water 50mL, weighed weight is added in precision, and close plug gently shakes up, and impregnates 25-
It 35 minutes, is heated to reflux 1 hour, takes out, be cooled to room temperature, then weighed weight, the weight of less loss, then accurate addition are supplied with water
Methanol 48ml, weighed weight, close plug gently shake up, and are ultrasonically treated 1 hour, take out, are cooled to room temperature, then weighed weight, use first
Alcohol supplies the weight of less loss, shakes up, and filters or is centrifuged, as test solution.
S4, it is measured；
It is accurate respectively to draw reference substance solution and each 10 μ l of test solution, inject liquid chromatograph, measurement to get.
Embodiment 2
In the embodiment of the present invention, a kind of pithecellobium clypearia method of inspection, comprising the following steps:
S1, gradient elution is carried out；
Using octadecylsilane chemically bonded silica as filler；It is flowing with 0.2% phosphoric acid solution using acetonitrile as mobile phase A
Phase B, the regulation according to the form below carry out gradient elution；Gallic acid, quercitin are weighed, gallic acid Detection wavelength is 270nm, Mongolian oak
Skin glycosides Detection wavelength is 350nm.Number of theoretical plate is calculated by gallic acid peak should be not less than 4000, should not be low by the calculating of quercitin peak
In 10000.
| Time (minute) | Mobile phase A (%) | Mobile phase B (%) |
| 0-15 | 5-25 | 95-75 |
| 15-25 | 25 | 75 |
| 25-27 | 25-30 | 75-70 |
| 27-40 | 30 | 70 |
S2, preparation reference substance solution；
Precision weighs quercitin reference substance 7mg, gallic acid reference substance 8mg, adds methanol that each gallic acid of 1ml is made
0.3mg, 15 μ g of quercitin mixed solution to get.
The system of S3, test solution；
This product powder 2g is taken, accurately weighed, water 50mL, weighed weight is added in precision, and close plug gently shakes up, and impregnates 30 points
Clock is heated to reflux 1 hour, is taken out, is cooled to room temperature, then weighed weight, and the weight of less loss, then accurate addition methanol are supplied with water
50ml, weighed weight, close plug gently shake up, and are ultrasonically treated 1 hour, take out, are cooled to room temperature, then weighed weight, are mended with methanol
The weight of sufficient less loss, shakes up, and filters or is centrifuged, as test solution.
S4, it is measured；
It is accurate respectively to draw reference substance solution and each 10 μ l of test solution, inject liquid chromatograph, measurement to get.
Embodiment 3
In the embodiment of the present invention, a kind of pithecellobium clypearia method of inspection, comprising the following steps:
S1, gradient elution is carried out；
Using octadecylsilane chemically bonded silica as filler；It is flowing with 0.2% phosphoric acid solution using acetonitrile as mobile phase A
Phase B, the regulation according to the form below carry out gradient elution；Gallic acid, quercitin are weighed, gallic acid Detection wavelength is 270nm, Mongolian oak
Skin glycosides Detection wavelength is 350nm.Number of theoretical plate is calculated by gallic acid peak should be not less than 4000, should not be low by the calculating of quercitin peak
In 10000；
| Time (minute) | Mobile phase A (%) | Mobile phase B (%) |
| 0-15 | 5-25 | 95-75 |
| 15-25 | 25 | 75 |
| 25-27 | 25-30 | 75-70 |
| 27-40 | 30 | 70 |
Product solution is shone in S2, preparation；
Precision weighs quercitin reference substance 10mg, gallic acid reference substance 10mg, adds methanol that each galla turcica of every 1.2ml is made
Sour 0.4mg, 20 μ g of quercitin mixed solution to get；
The system of S3, test solution；
This product powder 2.1g is taken, accurately weighed, water 50mL, weighed weight is added in precision, and close plug gently shakes up, dipping 35
Minute, it is heated to reflux 1 hour, takes out, be cooled to room temperature, then weighed weight, the weight of less loss, then accurate addition first are supplied with water
Alcohol 52ml, weighed weight, close plug gently shake up, and are ultrasonically treated 1 hour, take out, are cooled to room temperature, then weighed weight, use methanol
The weight for supplying less loss, shakes up, and filters or is centrifuged, as test solution；
S4, it is measured；
It is accurate respectively to draw reference substance solution and each 10 μ l of test solution, inject liquid chromatograph, measurement to get.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (7)
1. a kind of pithecellobium clypearia method of inspection, which comprises the following steps: S1, carry out gradient elution；S2, preparation
Reference substance solution；The system of S3, test solution；S4, it is measured, accurate absorption reference substance solution and test solution are each respectively
10 μ l, inject liquid chromatograph, measurement to get.
2. the pithecellobium clypearia method of inspection according to claim 1, which is characterized in that step S1 method is according to different ladders
Degree elutes filler, mobile phase A and Mobile phase B；Gallic acid, quercitin are weighed, gallic acid Detection wavelength is
270nm, quercitin Detection wavelength are 350nm；Number of theoretical plate is calculated by gallic acid peak is not less than 4000, calculates by quercitin peak
Not less than 10000.
3. the pithecellobium clypearia method of inspection according to claim 2, which is characterized in that in step S1, with octadecyl silicon
Alkane bonded silica gel is filler；Using acetonitrile as mobile phase A, using 0.2% phosphoric acid solution as Mobile phase B.
4. the pithecellobium clypearia method of inspection according to claim 3, which is characterized in that in step S1, different gradient difference
Are as follows:
Time is 0-15min, mobile phase A 5%-25%, Mobile phase B 95%-75%；
Time is 15-25min, mobile phase A 25%, Mobile phase B 57%；
Time is 25-27min, mobile phase A 25%-30%, Mobile phase B 75%-70%；
Time is 27-40min, mobile phase A 30%, Mobile phase B 70%.
5. the pithecellobium clypearia method of inspection according to claim 1, which is characterized in that step S2 is that precision weighs quercitin
Reference substance, gallic acid reference substance 4-10mg add methanol that each gallic acid 0.2-0.4mg of every 0.8-1.2ml, quercitin is made
The mixed solution of 10-20 μ g to get.
6. the pithecellobium clypearia method of inspection according to claim 5, which is characterized in that step S2 is that precision weighs quercitin
Reference substance 7mg, gallic acid reference substance 8mg add methanol that each gallic acid 0.3mg of 1ml, the mixing of 15 μ g of quercitin is made molten
Liquid to get.
7. the pithecellobium clypearia method of inspection according to claim 1, which is characterized in that step S3 is to take this product powder 1.9-
2.1g, accurately weighed, water 50mL, weighed weight is added in precision, and close plug gently shakes up, and impregnates 25-35 minutes, it is small to be heated to reflux 1
When, it takes out, is cooled to room temperature, then weighed weight, the weight of less loss, then accurate addition methanol 48-52ml are supplied with water, it is weighed heavy
Amount, close plug gently shake up, and are ultrasonically treated 1 hour, take out, are cooled to room temperature, then weighed weight, the weight of less loss is supplied with methanol
Amount, shakes up, filters or be centrifuged, as test solution.
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