CN109490433A - A kind of detection method of Loropetalum wood medicinal material and its pharmaceutical preparation - Google Patents
A kind of detection method of Loropetalum wood medicinal material and its pharmaceutical preparation Download PDFInfo
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- CN109490433A CN109490433A CN201811232648.6A CN201811232648A CN109490433A CN 109490433 A CN109490433 A CN 109490433A CN 201811232648 A CN201811232648 A CN 201811232648A CN 109490433 A CN109490433 A CN 109490433A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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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
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Abstract
Present invention relates particularly to the detection methods of a kind of Loropetalum wood medicinal material and its pharmaceutical preparation.It is characterized by: by high performance liquid chromatography, using chlorogenic acid as reference substance, by carrying out quantitative detection to the chlorogenic acid in Loropetalum wood, to determine the content of Loropetalum wood in Loropetalum wood drug；It can be used for accurate evaluation Loropetalum wood quality of medicinal material；It is combined by thin-layer chromatography and high performance liquid chromatography, using chlorogenic acid as reference substance, by carrying out quantitative detection to the chlorogenic acid in Loropetalum wood, to determine the content of Loropetalum wood in Loropetalum wood pharmaceutical preparation；The quality analysis that can also be used for detecting the preparation (Loropetalum wood granule etc.) produced using Loropetalum wood as raw material, can directly apply to the quality analysis of actual production process and product.
Description
Technical field
The present invention relates to Pharmaceutical Analysis detection technique fields, and in particular to the detection of a kind of Loropetalum wood medicinal material and its pharmaceutical preparation
Method.
Background technique
Loropetalum wood is usually shrub, it is dilute be dungarunga, up to 12 meters, 30 centimetres of diameter；Sprig has rust stellate hair.It produces in the Changjiang river
Downstream and its on the south, tropic of cancer northern area.North India is also distributed.It is born in hill and hills shrubbery more.Root, leaf,
Flowers and fruits can be used as medicine, and can solve thermal hemostasis, clearing and activating the channels and collaterals, astringing to arrest bleeding, clearing heat and detoxicating, antidiarrheal.Medicinal material has been that " Chinese Pharmacopoeia " is received
It carries.It is raw material using Loropetalum wood, has developed the related preparations products such as Loropetalum wood granule.
However, now for the correlative study of Loropetalum wood, it is relatively fewer for the research of Loropetalum wood medicinal ingredient, specifically for Loropetalum
The detection method of the wooden medicinal material, it is also less；Also, currently, the kind of the pharmaceutical preparation of Loropetalum wood is also relatively fewer in the market, thus,
Also few special detection methods dedicated for Loropetalum wood pharmaceutical preparation, are substantially and are carried out with some universal test methods to it
It tests and analyzes；Detection specificity in this way is poor, has been unable to meet the related request of the modernization of Chinese medicine.
It is now anxious in order to meet the related request of drug test of the modernization of Chinese medicine for Loropetalum wood medicinal material and its pharmaceutical preparation
Need to develop it is a kind of dedicated for detection Loropetalum wood medicinal material and its pharmaceutical preparation exclusive detection method, improve detection sensitivity and specially
Attribute more preferably meets the related request of the modernization of Chinese medicine.
Summary of the invention
For the shortcoming of the exclusive detection method of drug of current Loropetalum wood medicinal material and its pharmaceutical preparation, it is not able to satisfy the Chinese medicine modern times
Change the increasingly developed related request detected for Loropetalum wood medicinal material and its pharmaceutical preparation, it is an object of the present invention to provide a kind of Loropetalum wood medicinal materials
And its drug test method of pharmaceutical preparation, the Loropetalum wood medicinal material provided through the invention and its pharmaceutical preparation detection method, it can
The vacancy for filling up current Loropetalum wood medicinal material and its exclusive detection method missing of pharmaceutical preparation, improves detection precision, more preferably in satisfaction
The related request of medicine modernization.
In order to achieve the above objectives, the present invention is achieved by the following technical programs:
The detection method of a kind of Loropetalum wood medicinal material and its pharmaceutical preparation, with high performance liquid chromatography to the key in Loropetalum wood medicinal material
Ingredient chlorogenic acid carries out quantitative detection, to realize analysis and control to Loropetalum wood quality of medicinal material；With thin-layered chromatography and efficient liquid
Phase chromatography combination carries out qualitative and quantitative detection to the key component chlorogenic acid of Loropetalum wood in Loropetalum wood pharmaceutical preparation respectively, with reality
Now to the analysis and control of Loropetalum wood pharmaceutical preparation quality.
Preferably, the detection method of the Loropetalum wood medicinal material, using octadecylsilane chemically bonded silica as filler；With first
- 0.1% formic acid of alcohol (20~28:72~80) is mobile phase；Detection wavelength is 326nm；The sample solution of efficient liquid phase and control
Product preparation is: take chlorogenic acid reference substance appropriate, it is accurately weighed, and add methanol that solution of every 1ml containing 0.1mg is made to get reference substance
Solution；This product about 0.5g is taken, it is accurately weighed, it sets in 100ml stuffed conical flask, precision plus 75% methanol solution 50ml are weighed heavy
Amount ultrasonic extraction 30 minutes, is taken out, lets cool, then weighed weight, supply the weight of less loss, shake up to get test solution；It surveys
Determine method and draw reference substance solution 10ul and test solution 10ul to be accurate respectively, injects liquid chromatograph, measure to get Loropetalum
The wooden content.
It is highly preferred that the detection method of the Loropetalum wood medicinal material, using octadecylsilane chemically bonded silica as filler；With first
- 0.1% formic acid of alcohol (22~28:72~78) is mobile phase；Detection wavelength is 326nm；The sample solution of efficient liquid phase and control
Product preparation is: take chlorogenic acid reference substance appropriate, it is accurately weighed, and add methanol that solution of every 1ml containing 0.1mg is made to get reference substance
Solution；This product about 0.5g is taken, it is accurately weighed, it sets in 100ml stuffed conical flask, precision plus 75% methanol solution 50ml are weighed heavy
Amount ultrasonic extraction 30 minutes, is taken out, lets cool, then weighed weight, supply the weight of less loss, shake up to get test solution；It surveys
Determine method and draw reference substance solution 10ul and test solution 10ul to be accurate respectively, injects liquid chromatograph, measure to get Loropetalum
The wooden content.
Preferably, the qualitative checking method of the pharmaceutical preparation of the Loropetalum wood is to fill out with octadecylsilane chemically bonded silica
Fill agent；Using acetonitrile as mobile phase A, using 0.1 formic acid as Mobile phase B, and gradient elution is carried out；Detection wavelength is 326nm.Theoretical plate
By number of theoretical plate, the grate based on chlorogenic acid peak should be not less than 4000 to number；Sample solution and reference substance preparation are: taking chlorogenic acid reference substance
In right amount, accurately weighed, add methanol that solution of every 1ml containing 0.1mg is made to get reference substance solution；This product about 0.5g is taken, precision claims
It is fixed, it sets in 50ml stuffed conical flask, precision plus 75% methanol solution 25ml, weighed weight, takes out within ultrasonic extraction 30 minutes, put
It is cold, then weighed weight, the weight of less loss is supplied, is shaken up to get test solution；Thin-layer chromatography qualitative test method are as follows:
S1. test solution and reference substance solution are taken, is tested according to thin-layered chromatography, it is molten to draw test solution, reference substance
Each 2 μ l of liquid puts respectively on same polyamide film, with n-Butanol acetic acid-water (3~5:1~2:1~2) for solvent, opens up
It opens, takes out, dry, set and inspected under ultraviolet light 365nm, in sample chromatogram, at the position corresponding to the chromatogram of the reference substance, show phase
With the spot of color；
S2. this product 1g is taken, methanol 20ml is added, is ultrasonically treated 30 minutes, filtration, filtrate is steamed to 1ml, molten as test sample
Liquid.Bletilla control medicinal material 0.5g separately is taken, is made in the same way of control medicinal material solution.It is tested according to thin-layered chromatography, draws test solution 5
~10 μ l, 2 μ l of control medicinal material solution, put respectively on same silica gel g thin-layer plate, with cyclohexane-ethyl acetate-methanol (5~7:
2~4:1~2) it is solvent, it is unfolded, takes out, dry, spray is heated several minutes with ethanol solution of sulfuric acid at 105 DEG C, is examined under daylight
Depending on position corresponding with reference medicine chromatography, showing the spot of same color in sample chromatogram；
S3. this product 2g is taken, water 20ml is added, is ultrasonically treated 20 minutes, 2ml is taken to add methanol 2ml, is centrifuged, filtering takes 2ml to add
, there is white precipitate in 3-5 drop glacial acetic acid and drop ammonium oxalate test solution (3.5% ammonium oxalate), then plus hydrochloric acid 1-2 drop, precipitating disappearance；
S4. this product 2g is taken, methanol 25ml is added, is ultrasonically treated 30 minutes, filtration, filtrate is evaporated, and it is molten that residue adds water 10ml to make
Solution is saturated with water n-butanol shaking and extracts 2 times, each 20ml, merges n-butanol liquid, be washed with water 2~4 times, each 20ml, abandon
Aqueous is gone, n-butanol liquid is evaporated, and residue adds methanol 2ml to make to dissolve, as the another extracting liquorice control medicinal material lg of test solution, together
Control medicinal material solution extracting liquorice acid mono-ammonium reference substance again is made in method, adds methanol that solution of every lml containing 2mg is made, as control
Product solution is tested according to thin-layered chromatography, is drawn above-mentioned each 1~2 μ l of three kinds of solution, is put respectively molten with 1% sodium hydroxide in same
It is expansion with acetic ether-methanoic acid-glacial acetic acid-water (13~16:1~2:1~3:1~3) on the silica gel g thin-layer plate of liquid preparation
Agent is unfolded, and takes out, dries, and with 10% ethanol solution of sulfuric acid, it is clear to be heated to spot Xian Se Cheongju at 105 DEG C for spray, inspects under daylight
In sample chromatogram, on position corresponding with reference substance, reference medicine chromatography, the spot of same color is shown.
It is highly preferred that the qualitative checking method of the pharmaceutical preparation of the Loropetalum wood, is with octadecylsilane chemically bonded silica
Filler；Using acetonitrile as mobile phase A, using 0.1 formic acid as Mobile phase B, and gradient elution is carried out；Detection wavelength is 326nm.It is theoretical
By number of theoretical plate, the grate based on chlorogenic acid peak should be not less than 4000 to plate number；Sample solution and reference substance preparation are: chlorogenic acid being taken to compare
Appropriate product, it is accurately weighed, add methanol that solution of every 1ml containing 0.1mg is made to get reference substance solution；This product about 0.5g is taken, it is accurate
It is weighed, it sets in 50ml stuffed conical flask, precision plus 75% methanol solution 25ml, weighed weight, takes out within ultrasonic extraction 30 minutes, put
It is cold, then weighed weight, the weight of less loss is supplied, is shaken up to get test solution；Thin-layer chromatography qualitative test method are as follows:
S1. test solution and reference substance solution are taken, is tested according to thin-layered chromatography, it is molten to draw test solution, reference substance
Each 2 μ l of liquid is put respectively on same polyamide film, and with n-Butanol acetic acid-water (4~5:1:1) for solvent, expansion is taken
Out, it dries, sets and inspected under ultraviolet light 365nm, in sample chromatogram, at the position corresponding to the chromatogram of the reference substance, show identical face
The spot of color；
S2. this product 1g is taken, methanol 20ml is added, is ultrasonically treated 30 minutes, filtration, filtrate is steamed to 1ml, molten as test sample
Liquid.Bletilla control medicinal material 0.5g separately is taken, is made in the same way of control medicinal material solution.It is tested according to thin-layered chromatography, draws test solution 5
~10 μ l, 2 μ l of control medicinal material solution, put respectively on same silica gel g thin-layer plate, with cyclohexane-ethyl acetate-methanol (6~7:
2~3:1~2) it is solvent, it is unfolded, takes out, dry, spray is heated several minutes with ethanol solution of sulfuric acid at 105 DEG C, is examined under daylight
Depending on position corresponding with reference medicine chromatography, showing the spot of same color in sample chromatogram；
S3. this product 2g is taken, water 20ml is added, is ultrasonically treated 20 minutes, 2ml is taken to add methanol 2ml, is centrifuged, filtering takes 2ml to add
, there is white precipitate in 3-5 drop glacial acetic acid and drop ammonium oxalate test solution (3.5% ammonium oxalate), then plus hydrochloric acid 1-2 drop, precipitating disappearance；
S4. this product 2g is taken, methanol 25ml is added, is ultrasonically treated 30 minutes, filtration, filtrate is evaporated, and it is molten that residue adds water 10ml to make
Solution is saturated with water n-butanol shaking and extracts 2 times, each 20ml, merges n-butanol liquid, be washed with water 2~4 times, each 20ml, abandon
Aqueous is gone, n-butanol liquid is evaporated, and residue adds methanol 2ml to make to dissolve, as the another extracting liquorice control medicinal material lg of test solution, together
Control medicinal material solution extracting liquorice acid mono-ammonium reference substance again is made in method, adds methanol that solution of every lml containing 2mg is made, as control
Product solution is tested according to thin-layered chromatography, is drawn above-mentioned each 1~2 μ l of three kinds of solution, is put respectively molten with 1% sodium hydroxide in same
It is expansion with acetic ether-methanoic acid-glacial acetic acid-water (13~16:1~2:1~3:1~3) on the silica gel g thin-layer plate of liquid preparation
Agent is unfolded, and takes out, dries, and with 10% ethanol solution of sulfuric acid, it is clear to be heated to spot Xian Se Cheongju at 105 DEG C for spray, inspects under daylight
In sample chromatogram, on position corresponding with reference substance, reference medicine chromatography, the spot of same color is shown.
Preferably, the quantitative detecting method of the pharmaceutical preparation of the Loropetalum wood is to fill out with octadecylsilane chemically bonded silica
Fill agent；Using acetonitrile as mobile phase A, using 0.1 formic acid as Mobile phase B, and gradient elution is carried out；Detection wavelength is 326nm.Theoretical plate
Number, which is calculated by number of theoretical plate by chlorogenic acid peak, should be not less than 4000；Sample solution and reference substance preparation are: taking chlorogenic acid reference substance
In right amount, accurately weighed, add methanol that solution of every 1ml containing 0.1mg is made to get reference substance solution；This product about 0.5g is taken, precision claims
It is fixed, it sets in 50ml stuffed conical flask, precision plus 75% methanol solution 25ml, weighed weight, takes out within ultrasonic extraction 30 minutes, put
It is cold, then weighed weight, the weight of less loss is supplied, is shaken up to get test solution；Efficient liquid phase quantitative detecting method are as follows:
S1. using octadecylsilane chemically bonded silica as filler；Using acetonitrile as mobile phase A, using 0.1 formic acid as Mobile phase B,
Regulation according to the form below carries out gradient elution；Detection wavelength is 326nm.Number of theoretical plate by number of theoretical plate, answer by the grate based on chlorogenic acid peak
Not less than 4000；
S2. accurate respectively to draw reference substance solution 10ul and test solution 10ul, liquid chromatograph is injected, is measured, note
Chromatogram is recorded to get Loropetalum wood content.
Preferably, the preparation is the various preparations produced using Loropetalum wood as raw material, including Loropetalum wood granule, tablet, glue
Wafer, oral solution etc..
It is mainly the Western medicine system based on Western medicine preparation for the related drugs for treating gastric ulcer and its bleeding currently on the market
The advantages of agent is that analgesic is fast, but is easy recurrence；The opposite analgesic speed of Chinese materia medica preparation is slightly slow, but treating both manifestation and root cause of disease, is not easy
Recurrence is used to treat gastric ulcer currently on the market and its Chinese materia medica preparation of bleeding is relatively fewer, the equal energy of root, leaf, flowers and fruits of Loropetalum wood
It is used as medicine, there is solution thermal hemostasis, clearing and activating the channels and collaterals, astringing to arrest bleeding, clearing heat and detoxicating, the effect of antidiarrheal has not treatment gastric ulcer etc.
Wrong curative effect is had a vast market foreground and commercial value with developing relevant Chinese materia medica preparation.
But with the requirement of the modernization of Chinese medicine, the detection of relevant Chinese herb and preparation is proposed higher
Requirement, it is desirable that develop its exclusive detection method with improve its detection accuracy and precision；But Loropetalum wood medicinal material and its medicine
The exclusive detection method of object preparation is still short of；The exclusive detection method energy of Loropetalum wood medicinal material and its pharmaceutical preparation provided by the invention
Enough related requests for more preferably meeting the modernization of Chinese medicine, improve the precision and accuracy of detection.
Specific embodiment
The present invention is further elaborated combined with specific embodiments below, the embodiment is served only for explaining this hair
It is bright, it is not intended to limit the scope of the present invention.Test method as used in the following examples is routine unless otherwise specified
Method；Used material, reagent etc., unless otherwise specified, for the reagent and material commercially obtained.
Embodiment 1
The white flower loropetalum chinense qualitative checking method of the pharmaceutical preparation of Loropetalum wood, using octadecylsilane chemically bonded silica as filler；
Using acetonitrile as mobile phase A, using 0.1 formic acid as Mobile phase B, and gradient elution is carried out；Detection wavelength is 326nm.Number of theoretical plate is pressed
Number of theoretical plate grate based on chlorogenic acid peak should be not less than 4000；Sample solution and reference substance preparation are: take chlorogenic acid reference substance appropriate,
It is accurately weighed, add methanol that solution of every 1ml containing 0.1mg is made to get reference substance solution；This product about 0.5g is taken, it is accurately weighed, it sets
In 50ml stuffed conical flask, precision plus 75% methanol solution 25ml, weighed weight are taken out, are let cool, then claim for ultrasonic extraction 30 minutes
Determine weight, supplies the weight of less loss, shake up to get test solution；Thin-layer chromatography qualitative test method are as follows:
S1. test solution and reference substance solution are taken, is tested according to thin-layered chromatography, it is molten to draw test solution, reference substance
Each 2 μ l of liquid puts respectively on same polyamide film, with n-Butanol acetic acid-water (3:1:1) for solvent, is unfolded, takes out, dry in the air
It is dry, it sets and is inspected under ultraviolet light 365nm, in sample chromatogram, at the position corresponding to the chromatogram of the reference substance, show the spot of same color
Point；
S2. this product 1g is taken, methanol 20ml is added, is ultrasonically treated 30 minutes, filtration, filtrate is steamed to 1ml, molten as test sample
Liquid.Bletilla control medicinal material 0.5g separately is taken, is made in the same way of control medicinal material solution.It is tested according to thin-layered chromatography, draws test solution 5
~10 μ l, 2 μ l of control medicinal material solution, put respectively on same silica gel g thin-layer plate, with cyclohexane-ethyl acetate-methanol (5:3:
1) it is solvent, is unfolded, take out, dry, spray is heated several minutes with ethanol solution of sulfuric acid at 105 DEG C, is inspected under daylight, for examination
In product chromatography, on position corresponding with reference medicine chromatography, the spot of same color is shown；
S3. this product 2g is taken, water 20ml is added, is ultrasonically treated 20 minutes, 2ml is taken to add methanol 2ml, is centrifuged, filtering takes 2ml to add
, there is white precipitate in 3-5 drop glacial acetic acid and drop ammonium oxalate test solution (3.5% ammonium oxalate), then plus hydrochloric acid 1-2 drop, precipitating disappearance；
S4. this product 2g is taken, methanol 25ml is added, is ultrasonically treated 30 minutes, filtration, filtrate is evaporated, and it is molten that residue adds water 10ml to make
Solution is saturated with water n-butanol shaking and extracts 2 times, each 20ml, merges n-butanol liquid, be washed with water 2~4 times, each 20ml, abandon
Aqueous is gone, n-butanol liquid is evaporated, and residue adds methanol 2ml to make to dissolve, as the another extracting liquorice control medicinal material lg of test solution, together
Control medicinal material solution extracting liquorice acid mono-ammonium reference substance again is made in method, adds methanol that solution of every lml containing 2mg is made, as control
Product solution is tested according to thin-layered chromatography, is drawn above-mentioned each 1~2 μ l of three kinds of solution, is put respectively molten with 1% sodium hydroxide in same
On the silica gel g thin-layer plate of liquid preparation, with acetic ether-methanoic acid-glacial acetic acid-water (13:1:1:1) for solvent, it is unfolded, takes out,
It dries, with 10% ethanol solution of sulfuric acid, it is clear to be heated to spot Xian Se Cheongju at 105 DEG C for spray, it is inspected under daylight in sample chromatogram,
On position corresponding with reference substance, reference medicine chromatography, the spot of same color is shown.
The quantitative detecting method of white flower loropetalum chinense in the pharmaceutical preparation of Loropetalum wood is filling with octadecylsilane chemically bonded silica
Agent；Using acetonitrile as mobile phase A, using 0.1 formic acid as Mobile phase B, and gradient elution is carried out；Detection wavelength is 326nm.Number of theoretical plate
4000 should be not less than by calculating by number of theoretical plate by chlorogenic acid peak；Sample solution and reference substance preparation are: taking chlorogenic acid reference substance suitable
Amount, it is accurately weighed, add methanol that solution of every 1ml containing 0.1mg is made to get reference substance solution；This product about 0.5g is taken, precision claims
It is fixed, it sets in 50ml stuffed conical flask, precision plus 75% methanol solution 25ml, weighed weight, takes out within ultrasonic extraction 30 minutes, put
It is cold, then weighed weight, the weight of less loss is supplied, is shaken up to get test solution；Efficient liquid phase quantitative detecting method are as follows:
S1. using octadecylsilane chemically bonded silica as filler；Using acetonitrile as mobile phase A, using 0.1 formic acid as Mobile phase B,
Regulation according to the form below carries out gradient elution；Detection wavelength is 326nm.Number of theoretical plate by number of theoretical plate, answer by the grate based on chlorogenic acid peak
Not less than 4000；
S2. accurate respectively to draw reference substance solution 10ul and test solution 10ul, liquid chromatograph is injected, is measured, note
Chromatogram is recorded to get Loropetalum wood content.
The detection method of white flower loropetalum chinense content in Loropetalum wood medicinal material, using octadecylsilane chemically bonded silica as filler；With first
- 0.1% formic acid of alcohol (20:72) is mobile phase；Detection wavelength is 326nm；Sample solution and the reference substance preparation of efficient liquid phase are:
Take chlorogenic acid reference substance appropriate, it is accurately weighed, add methanol that solution of every 1ml containing 0.1mg is made to get reference substance solution；Take this
Product about 0.5g, it is accurately weighed, it sets in 100ml stuffed conical flask, precision plus 75% methanol solution 50ml, weighed weight, ultrasound mentions
It takes 30 minutes, takes out, let cool, then weighed weight, supply the weight of less loss, shake up to get test solution；Measuring method is point
It is inaccurate to draw reference substance solution 10ul and test solution 10ul, liquid chromatograph is injected, is measured to get Loropetalum wood content.
Embodiment 2
White flower loropetalum chinense qualitative checking method in the pharmaceutical preparation of Loropetalum wood is filling with octadecylsilane chemically bonded silica
Agent；Using acetonitrile as mobile phase A, using 0.1 formic acid as Mobile phase B, and gradient elution is carried out；Detection wavelength is 326nm.Number of theoretical plate
By number of theoretical plate, grate should be not less than 4000 based on chlorogenic acid peak；Sample solution and reference substance preparation are: taking chlorogenic acid reference substance suitable
Amount, it is accurately weighed, add methanol that solution of every 1ml containing 0.1mg is made to get reference substance solution；This product about 0.5g is taken, precision claims
It is fixed, it sets in 50ml stuffed conical flask, precision plus 75% methanol solution 25ml, weighed weight, takes out within ultrasonic extraction 30 minutes, put
It is cold, then weighed weight, the weight of less loss is supplied, is shaken up to get test solution；Thin-layer chromatography qualitative test method are as follows:
S1. test solution and reference substance solution are taken, is tested according to thin-layered chromatography, it is molten to draw test solution, reference substance
Each 2 μ l of liquid puts respectively on same polyamide film, with n-Butanol acetic acid-water (5:2:2) for solvent, is unfolded, takes out, dry in the air
It is dry, it sets and is inspected under ultraviolet light 365nm, in sample chromatogram, at the position corresponding to the chromatogram of the reference substance, show the spot of same color
Point；
S2. this product 1g is taken, methanol 20ml is added, is ultrasonically treated 30 minutes, filtration, filtrate is steamed to 1ml, molten as test sample
Liquid.Bletilla control medicinal material 0.5g separately is taken, is made in the same way of control medicinal material solution.It is tested according to thin-layered chromatography, draws test solution 5
~10 μ l, 2 μ l of control medicinal material solution, put respectively on same silica gel g thin-layer plate, with cyclohexane-ethyl acetate-methanol (6:4:
1) it is solvent, is unfolded, take out, dry, spray is heated several minutes with ethanol solution of sulfuric acid at 105 DEG C, is inspected under daylight, for examination
In product chromatography, on position corresponding with reference medicine chromatography, the spot of same color is shown；
S3. this product 2g is taken, water 20ml is added, is ultrasonically treated 20 minutes, 2ml is taken to add methanol 2ml, is centrifuged, filtering takes 2ml to add
, there is white precipitate in 3-5 drop glacial acetic acid and drop ammonium oxalate test solution (3.5% ammonium oxalate), then plus hydrochloric acid 1-2 drop, precipitating disappearance；
S4. this product 2g is taken, methanol 25ml is added, is ultrasonically treated 30 minutes, filtration, filtrate is evaporated, and it is molten that residue adds water 10ml to make
Solution is saturated with water n-butanol shaking and extracts 2 times, each 20ml, merges n-butanol liquid, be washed with water 2~4 times, each 20ml, abandon
Aqueous is gone, n-butanol liquid is evaporated, and residue adds methanol 2ml to make to dissolve, as the another extracting liquorice control medicinal material lg of test solution, together
Control medicinal material solution extracting liquorice acid mono-ammonium reference substance again is made in method, adds methanol that solution of every lml containing 2mg is made, as control
Product solution is tested according to thin-layered chromatography, is drawn above-mentioned each 1~2 μ l of three kinds of solution, is put respectively molten with 1% sodium hydroxide in same
On the silica gel g thin-layer plate of liquid preparation, with acetic ether-methanoic acid-glacial acetic acid-water (15:2:3:3) for solvent, it is unfolded, takes out,
It dries, with 10% ethanol solution of sulfuric acid, it is clear to be heated to spot Xian Se Cheongju at 105 DEG C for spray, it is inspected under daylight in sample chromatogram,
On position corresponding with reference substance, reference medicine chromatography, the spot of same color is shown.
The quantitative detecting method of white flower loropetalum chinense in the pharmaceutical preparation of Loropetalum wood is filling with octadecylsilane chemically bonded silica
Agent；Using acetonitrile as mobile phase A, using 0.1 formic acid as Mobile phase B, and gradient elution is carried out；Detection wavelength is 326nm.Number of theoretical plate
4000 should be not less than by calculating by number of theoretical plate by chlorogenic acid peak；Sample solution and reference substance preparation are: taking chlorogenic acid reference substance suitable
Amount, it is accurately weighed, add methanol that solution of every 1ml containing 0.1mg is made to get reference substance solution；This product about 0.5g is taken, precision claims
It is fixed, it sets in 50ml stuffed conical flask, precision plus 75% methanol solution 25ml, weighed weight, takes out within ultrasonic extraction 30 minutes, put
It is cold, then weighed weight, the weight of less loss is supplied, is shaken up to get test solution；Efficient liquid phase quantitative detecting method are as follows:
S1. using octadecylsilane chemically bonded silica as filler；Using acetonitrile as mobile phase A, using 0.1 formic acid as Mobile phase B,
Regulation according to the form below carries out gradient elution；Detection wavelength is 326nm.Number of theoretical plate by number of theoretical plate, answer by the grate based on chlorogenic acid peak
Not less than 4000；
S2. accurate respectively to draw reference substance solution 10ul and test solution 10ul, liquid chromatograph is injected, is measured, note
Chromatogram is recorded to get Loropetalum wood content.
The detection method of white flower loropetalum chinense in Loropetalum wood medicinal material, using octadecylsilane chemically bonded silica as filler；With methanol-
0.1% formic acid (27:78) is mobile phase；Detection wavelength is 326nm；Sample solution and the reference substance preparation of efficient liquid phase are: taking
Chlorogenic acid reference substance is appropriate, accurately weighed, adds methanol that solution of every 1ml containing 0.1mg is made to get reference substance solution；Take this product
About 0.5g, it is accurately weighed, it sets in 100ml stuffed conical flask, precision plus 75% methanol solution 50ml, weighed weight, ultrasonic extraction
It 30 minutes, takes out, lets cool, then weighed weight, supply the weight of less loss, shake up to get test solution；Measuring method is difference
Precision draws reference substance solution 10ul and test solution 10ul, injects liquid chromatograph, measures to get Loropetalum wood content.
1. stability test
Take same batch of sample (lot number) that test solution is made by text method, precision draws same 10 μ of test solution
L is measured in accordance with the law 0 after preparation, 1,2,4,8,24 hours, the results showed that, test solution is substantially steady in 24 hours
It is fixed.It the results are shown in Table 1.
1 stability test of table
2. precision test
Take same batch of sample that test solution is made by text method, precision is drawn same test solution, determined
HPLC under the conditions of, 10 μ l of sample introduction, repeat sample introduction 5 times, acquire chlorogenic acid peak area relative standard deviation < 2%, the results are shown in Table
2。
2 precision test of table
3. repetitive test
Text method is pressed, same batch 6 parts of sample are measured, under the conditions of identified HPLC, is measured, as a result
It is shown in Table 3, relative standard deviation < 3%, illustration method reproducibility is good.
3 repetitive test of table
4. recovery test
Using sample-adding absorption method, precision weighs the sample (lot number, content 6.836mg/g) of the same lot number of known content
0.25g, it is accurate respectively that chlorogenic acid (0.0386mg/ml) 75% methanol solution 50ml is added, by the preparation of text test solution
The rate of recovery is calculated as follows in method preparation and above-mentioned chromatographic condition, measurement, and as a result average recovery rate chlorogenic acid is 99.78, relatively
Standard deviation is 1.28%, and illustration method is reliably, to the results are shown in Table 4.
4 recovery test of table
5. sample measurement test
By the content of method measurement chlorogenic acid in embodiment, it the results are shown in Table 5
5 sample measurement result of table
Finally it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than the present invention is protected
The limitation of range is protected, although explaining in detail referring to preferred embodiment to the present invention, those skilled in the art are answered
Work as understanding, it can be with modification or equivalent replacement of the technical solution of the present invention are made, without departing from the reality of technical solution of the present invention
Matter and range.
Claims (7)
1. the detection method of a kind of Loropetalum wood medicinal material and its pharmaceutical preparation, which is characterized in that with high performance liquid chromatography to Loropetalum wood medicine
Key component chlorogenic acid in material carries out quantitative detection, to realize analysis and control to Loropetalum wood quality of medicinal material；With thin-layer chromatography
Method and high performance liquid chromatography combination respectively carry out the key component chlorogenic acid of Loropetalum wood in Loropetalum wood pharmaceutical preparation qualitative and quantitative
Detection, to realize analysis and control to Loropetalum wood pharmaceutical preparation quality.
2. the detection method of Loropetalum wood medicinal material according to claim 1, using octadecylsilane chemically bonded silica as filler；With
- 0.1% formic acid of methanol (20~28:72~80) is mobile phase；Detection wavelength is 326nm；The sample solution of efficient liquid phase and right
It is according to product preparation: takes chlorogenic acid reference substance appropriate, it is accurately weighed, add methanol that solution of every 1ml containing 0.1mg is made to get control
Product solution；This product about 0.5g is taken, it is accurately weighed, it sets in 100ml stuffed conical flask, precision plus 75% methanol solution 50ml are weighed
Weight ultrasonic extraction 30 minutes, is taken out, lets cool, then weighed weight, supply the weight of less loss, shake up to get test solution；
Measuring method be it is accurate respectively draw reference substance solution 10ul and test solution 10ul, inject liquid chromatograph, measurement to get
Loropetalum wood content.
3. the qualitative checking method of the pharmaceutical preparation of Loropetalum wood according to claim 1, with octadecylsilane chemically bonded silica
For filler；Using acetonitrile as mobile phase A, using 0.1 formic acid as Mobile phase B, and gradient elution is carried out；Detection wavelength is 326nm.Reason
By plate number, by number of theoretical plate, the grate based on chlorogenic acid peak should be not less than 4000；Sample solution and reference substance preparation are: taking chlorogenic acid pair
It is appropriate according to product, it is accurately weighed, add methanol that solution of every 1ml containing 0.1mg is made to get reference substance solution；This product about 0.5g is taken, essence
It is close weighed, it sets in 50ml stuffed conical flask, precision plus 75% methanol solution 25ml, weighed weight, takes out within ultrasonic extraction 30 minutes,
It lets cool, then weighed weight, supplies the weight of less loss, shake up to get test solution；Thin-layer chromatography qualitative test method are as follows:
S1. test solution and reference substance solution are taken, is tested according to thin-layered chromatography, test solution, reference substance solution each 2 are drawn
μ l is put respectively on same polyamide film, and with n-Butanol acetic acid-water (3~5:1~2:1~2) for solvent, expansion is taken
Out, it dries, sets and inspected under ultraviolet light 365nm, in sample chromatogram, at the position corresponding to the chromatogram of the reference substance, show identical face
The spot of color；
S2. this product 1g is taken, methanol 20m l is added, is ultrasonically treated 30 minutes, filtration, filtrate is steamed to 1ml, as test solution.Separately
Bletilla control medicinal material 0.5g is taken, control medicinal material solution is made in the same way of.It is tested according to thin-layered chromatography, draws 5~10 μ of test solution
L, 2 μ l of control medicinal material solution, puts respectively on same silica gel g thin-layer plate, with cyclohexane-ethyl acetate-methanol (5~7:2~4:
1~2) it is solvent, is unfolded, take out, dry, spray is heated several minutes with ethanol solution of sulfuric acid at 105 DEG C, is inspected under daylight, is supplied
In test product chromatography, on position corresponding with reference medicine chromatography, the spot of same color is shown；
S3. this product 2g is taken, water 20m l is added, is ultrasonically treated 20 minutes, 2ml is taken to add methanol 2ml, is centrifuged, filtering takes 2ml to add 3-5
Drip glacial acetic acid and drop ammonium oxalate test solution (3.5% ammonium oxalate), white precipitate occur, then plus hydrochloric acid 1-2 drop, precipitating disappearance；
S4. this product 2g is taken, methanol 25m l is added, is ultrasonically treated 30 minutes, filtration, filtrate is evaporated, and residue adds water 10ml to make to dissolve,
It is saturated with water n-butanol shaking to extract 2 times, each 20ml, merges n-butanol liquid, be washed with water 2~4 times, each 20ml is discarded
Aqueous, n-butanol liquid are evaporated, and residue adds methanol 2ml to make to dissolve, as the another extracting liquorice control medicinal material lg of test solution, same to method
Control medicinal material solution extracting liquorice acid mono-ammonium reference substance again is made, adds methanol that every solution of the lm l containing 2mg is made, as control
Product solution is tested according to thin-layered chromatography, is drawn above-mentioned each 1~2 μ l of three kinds of solution, is put respectively molten with 1% sodium hydroxide in same
It is expansion with acetic ether-methanoic acid-glacial acetic acid-water (13~16:1~2:1~3:1~3) on the silica gel g thin-layer plate of liquid preparation
Agent is unfolded, and takes out, dries, and with 10% ethanol solution of sulfuric acid, it is clear to be heated to spot Xian Se Cheongju at 105 DEG C for spray, inspects under daylight
In sample chromatogram, on position corresponding with reference substance, reference medicine chromatography, the spot of same color is shown.
4. the quantitative detecting method of the pharmaceutical preparation of Loropetalum wood according to claim 1, with octadecylsilane chemically bonded silica
For filler；Using acetonitrile as mobile phase A, using 0.1 formic acid as Mobile phase B, and gradient elution is carried out；Detection wavelength is 326nm.Reason
4000 should be not less than by calculating by number of theoretical plate by chlorogenic acid peak by plate number；Sample solution and reference substance preparation are: taking chlorogenic acid pair
It is appropriate according to product, it is accurately weighed, add methanol that solution of every 1ml containing 0.1mg is made to get reference substance solution；This product about 0.5g is taken, essence
It is close weighed, it sets in 50ml stuffed conical flask, precision plus 75% methanol solution 25ml, weighed weight, takes out within ultrasonic extraction 30 minutes,
It lets cool, then weighed weight, supplies the weight of less loss, shake up to get test solution；Efficient liquid phase quantitative detecting method are as follows:
S1. using octadecylsilane chemically bonded silica as filler；Using acetonitrile as mobile phase A, using 0.1 formic acid as Mobile phase B, press
Regulation in table carries out gradient elution；Detection wavelength is 326nm.Grate should not be low based on chlorogenic acid peak by number of theoretical plate for number of theoretical plate
In 4000；
S2. accurate respectively to draw reference substance solution 10ul and test solution 10ul, liquid chromatograph is injected, measurement records color
Spectrogram is to get Loropetalum wood content.
5. according to wooden dose of detection method of Loropetalum described in claim 1, it is characterised in that: the preparation is using Loropetalum wood as raw material
The various preparations, including Loropetalum wood granule, tablet, capsule, oral solution etc. of production.
6. the detection method of Loropetalum wood medicinal material according to claim 2, which is characterized in that with octadecylsilane chemically bonded silica
For filler；With -0.1% formic acid of methanol (20~25:75~80) for mobile phase；Detection wavelength is 326nm；The sample of efficient liquid phase
Product solution and reference substance preparation are: take chlorogenic acid reference substance appropriate, it is accurately weighed, and add methanol that every 1ml is made containing the molten of 0.1mg
Liquid is to get reference substance solution；This product about 0.5g is taken, it is accurately weighed, it sets in 100ml stuffed conical flask, precision plus 75% methanol are molten
Liquid 50ml, weighed weight, ultrasonic extraction 30 minutes, take out, let cool, then weighed weight, supply the weight of less loss, shake up to get
Test solution；Measuring method is that precision draws reference substance solution 10ul and test solution 10ul respectively, injects liquid chromatogram
Instrument measures to get Loropetalum wood content.
7. the qualitative checking method of the pharmaceutical preparation of Loropetalum wood according to claim 3, with octadecylsilane chemically bonded silica
For filler；Using acetonitrile as mobile phase A, using 0.1 formic acid as Mobile phase B, and gradient elution is carried out；Detection wavelength is 326nm.Reason
By plate number, by number of theoretical plate, the grate based on chlorogenic acid peak should be not less than 4000；Sample solution and reference substance preparation are: taking chlorogenic acid pair
It is appropriate according to product, it is accurately weighed, add methanol that solution of every 1ml containing 0.1mg is made to get reference substance solution；This product about 0.5g is taken, essence
It is close weighed, it sets in 50ml stuffed conical flask, precision plus 75% methanol solution 25ml, weighed weight, takes out within ultrasonic extraction 30 minutes,
It lets cool, then weighed weight, supplies the weight of less loss, shake up to get test solution；Thin-layer chromatography qualitative test method are as follows:
S1. test solution and reference substance solution are taken, is tested according to thin-layered chromatography, test solution, reference substance solution each 2 are drawn
μ l puts respectively on same polyamide film, with n-Butanol acetic acid-water (4~5:1:1) for solvent, is unfolded, takes out, dry in the air
It is dry, it sets and is inspected under ultraviolet light 365nm, in sample chromatogram, at the position corresponding to the chromatogram of the reference substance, show the spot of same color
Point；
S2. this product 1g is taken, methanol 20m l is added, is ultrasonically treated 30 minutes, filtration, filtrate is steamed to 1ml, as test solution.Separately
Bletilla control medicinal material 0.5g is taken, control medicinal material solution is made in the same way of.It is tested according to thin-layered chromatography, draws 5~10 μ of test solution
L, 2 μ l of control medicinal material solution, puts respectively on same silica gel g thin-layer plate, with cyclohexane-ethyl acetate-methanol (6~7:2~3:
1~2) it is solvent, is unfolded, take out, dry, spray is heated several minutes with ethanol solution of sulfuric acid at 105 DEG C, is inspected under daylight, is supplied
In test product chromatography, on position corresponding with reference medicine chromatography, the spot of same color is shown；
S3. this product 2g is taken, water 20m l is added, is ultrasonically treated 20 minutes, 2ml is taken to add methanol 2ml, is centrifuged, filtering takes 2ml to add 3-5
Drip glacial acetic acid and drop ammonium oxalate test solution (3.5% ammonium oxalate), white precipitate occur, then plus hydrochloric acid 1-2 drop, precipitating disappearance；
S4. this product 2g is taken, methanol 25m l is added, is ultrasonically treated 30 minutes, filtration, filtrate is evaporated, and residue adds water 10ml to make to dissolve,
It is saturated with water n-butanol shaking to extract 2 times, each 20ml, merges n-butanol liquid, be washed with water 2~4 times, each 20ml is discarded
Aqueous, n-butanol liquid are evaporated, and residue adds methanol 2ml to make to dissolve, as the another extracting liquorice control medicinal material lg of test solution, same to method
Control medicinal material solution extracting liquorice acid mono-ammonium reference substance again is made, adds methanol that every solution of the lm l containing 2mg is made, as control
Product solution is tested according to thin-layered chromatography, is drawn above-mentioned each 1~2 μ l of three kinds of solution, is put respectively molten with 1% sodium hydroxide in same
It is expansion with acetic ether-methanoic acid-glacial acetic acid-water (13~16:1~2:1~3:1~3) on the silica gel g thin-layer plate of liquid preparation
Agent is unfolded, and takes out, dries, and with 10% ethanol solution of sulfuric acid, it is clear to be heated to spot Xian Se Cheongju at 105 DEG C for spray, inspects under daylight
In sample chromatogram, on position corresponding with reference substance, reference medicine chromatography, the spot of same color is shown.
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Effective date of registration: 20191223 Address after: Room 106-1002, building 2, yard 8, Xingsheng South Road, Miyun District, Beijing Applicant after: Beijing Loropetalum chinense Biotechnology Co., Ltd Address before: 215500 No. 1, 22 Blocks, Four Districts, Wuxing New Village, Yushan Town, Changshu City, Jiangsu Province Applicant before: Liu Yunbin |
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