CN103063798A - Novel method for detecting Longdan Xiegan particles - Google Patents
Novel method for detecting Longdan Xiegan particles Download PDFInfo
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- CN103063798A CN103063798A CN2013100001974A CN201310000197A CN103063798A CN 103063798 A CN103063798 A CN 103063798A CN 2013100001974 A CN2013100001974 A CN 2013100001974A CN 201310000197 A CN201310000197 A CN 201310000197A CN 103063798 A CN103063798 A CN 103063798A
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Abstract
The invention relates to a novel method for detecting Longdan Xiegan particles and belongs to the field of modernization of Chinese traditional medicine. According to the invention, by establishment of identification and content determination on gentian serving as monarch drug and baical skullcap root serving as ministerial drug and content determination on gardenia, and being matched with original identification on gardenia, ingredients of the medicament and compatibility of the ingredients can be more comprehensively detected; the method for detecting the Longdan Xiegan particles is standardized; and the novel method is helpful to knowing content and stability of the Longdan Xiegan particles and explaining the medicinal material basis of the medicament.
Description
Technical field
The invention belongs to modern Chinese traditional medicine field, be specifically related to a kind of detection method of Longdanxiegan particle.
Background technology
Traditional Chinese medicine ingredients is complicated, and particularly Chinese medicine compound prescription often contains multiclass, Multiple components, has consisted of a very complicated system.At present, new active component Chinese medicine preparation and the research and development of modern Chinese traditional compound medicine are on the increase, and new technique and multiple different extracting mode also are used for research and the production of medicine.
Along with the fast development of Modern Testing, equipment and instrument, the assay of Chinese medicine, chromatographic identification become the important means of detection.But assay or the discriminating of at present generally only setting up a certain index chemical constitution for the simultaneously applied situation of above-mentioned multiple new technology, are only set up the assay of certain single component or are differentiated to a great extent with larger one-sidedness.
The Longdanxiegan particle has the clearing liver courage, the function of dampness removing heat.Be used for liver and gallbladder damp-heat, dizziness and red eyes, Hiccough and deaf, the ear pain that swells, the hypochondriac pain bitter taste is urinated red puckery pain, under the humid tropics.
The Longdanxiegan particle is yellow to tan particle; The little perfume (or spice) of gas, the flavor sweet, little hardship.
Its prescription is: rough gentian 66g, radix bupleuri 66g, root of large-flowered skullcap 33g, cape jasmine (stir-fry) 33g, rhizoma alismatis 66g, akebi 33g, plantain seed (salt stir-fry) 33g, Radix Angelicae Sinensis (wine stir-fry) 33g, glutinous rehmannia 66g, Radix Glycyrrhizae (honey is processed) 33g.
Method for making: above ten flavors, get radix bupleuri, Radix Angelicae Sinensis extraction volatile oil, the aqueous solution after the distillation in addition device is collected; Eight flavors such as the dregs of a decoction and all the other rough gentian, the boiling secondary adds 8 times of water gagings for the first time, decocts 1.5 hours, for the second time add 6 times of water gagings, decocted collecting decoction 1.5 hours, filter, filtrate and the merging of above-mentioned aqueous solution are concentrated into relative density and are 1.25～1.30(50～55 ℃) clear cream.1 part of qinghuo reagent, 2.5 parts of sucrose, 2 parts in dextrin and appropriate amount of ethanol, granulation, drying adds the volatile oil of above-mentioned radix bupleuri, Radix Angelicae Sinensis, and mixing is made 1000g, and get final product.Every packed 6g; Boiling water is taken after mixing it with water, a 6g, 2 times on the one.
Rough gentian rushes down the heat of the moon of fainting in the side, is monarch drug in a prescription, and the heat of the root of large-flowered skullcap, cape jasmine clearing lung-heat and three warmers to be helping it, and rhizoma alismatis rushes down that kidney channel is wet, and it is to be ministerial drug to help it that akebi, plantain seed are rushed down the wet of small intestine bladder, so medicines of dropping of bitter cold all.So with Radix Angelicae Sinensis, the dried rhizome of rehmannia to nourish blood tonifying liver, be adjutant altogether, with Radix Glycyrrhizae with in slow and do not make and injure one's stomach, for making medicine also.
Only has the discriminating to the ministerial drug cape jasmine in the original detection method of Longdanxiegan particle, but the monarch drug in a prescription role also is very important in the well-known side, as do not have corresponding detection means to cause easily detection method with larger one-sidedness, only content that can not comprehensively reflect the important composition of Longdanxiegan particle to the discriminating of cape jasmine of while.
Summary of the invention
The invention provides a kind of new detection method of Longdanxiegan particle
,To solve the problem that monarch drug in a prescription is not detected that exists in the present detection method.
The technical scheme that the present invention takes is to comprise following discrimination method and content assaying method:
(1) discrimination method
(1) get this product Longdanxiegan particle 12g, porphyrize adds methyl alcohol 50ml, adds hot reflux 1 hour, filter, filtrate evaporate to dryness, residue add water 15ml, and heating makes dissolving, let cool, the full normal butyl alcohol that closes of water extracts 2 times, and each 15ml merges n-butanol extracting liquid, the recovered under reduced pressure normal butyl alcohol is to doing, and residue adds methyl alcohol 2ml makes dissolving, is added on the neutral alumina column of having handled well, the neutral alumina that fills 120 orders, 2g, column internal diameter 15mm, with methyl alcohol 20ml wash-out, eluent is concentrated into 2ml, as need testing solution;
Other gets the gentiamarin reference substance, adds methyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution;
According to the test of an appendix VI of Chinese Pharmacopoeia version in 2005 B thin-layered chromatography, draw each 3 μ l of above-mentioned two kinds of solution, put in same silica G F respectively
254On the thin layer plate, with chloroform: methyl alcohol: water=13:6:2, lower floor's solution of placing below 10 ℃ is developping agent, launches, take out, dry, put inspection knowledge under the 254nm ultraviolet lamp, in the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color;
(2) get this product Longdanxiegan particle 12g, add water 30ml, heating makes dissolving, let cool, use extracted by ether 3 times, each 15ml, discard ether solution, the full normal butyl alcohol that closes of water extracts 3 times again, each 15ml, merge normal butyl alcohol liquid, add the equal-volume ammonia solution, shake up, place layering, divide and get supernatant, the recovered under reduced pressure normal butyl alcohol is to doing, residue adds methyl alcohol 1ml makes dissolving, as need testing solution; Other gets the Gardenoside reference substance, adds methyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; Thin-layered chromatography test with reference to an appendix VI of Chinese Pharmacopoeia version in 2005 B, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, take ethyl acetate: acetone: formic acid: water=5:5:1:1 launches as developping agent, takes out, dry, spray is with ethanol solution of sulfuric acid, and is about 10 minutes of 110 ℃ of bakings, clear to the spot colour developing; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color;
(3) get this product Longdanxiegan particle 12g, porphyrize adds methyl alcohol 50ml, add hot reflux 1 hour, and filtered the filtrate evaporate to dryness, residue adds water 15ml, and heating makes dissolving, lets cool, the full normal butyl alcohol that closes of water extracts 2 times, each 15ml merges n-butanol extracting liquid, and the recovered under reduced pressure normal butyl alcohol is to doing, residue adds methyl alcohol 2ml makes dissolving, as need testing solution; Other gets the scutelloside reference substance, adds methyl alcohol and makes the solution that every 1ml contains 5mg, in contrast product solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin-layered chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, take ethyl acetate: butanone: formic acid: water=5:3:1.1:1 is as developping agent, launch, take out, dry, spray is with 5% ferric trichloride ethanolic solution; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color;
(2) content assaying method
(1) according to an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring;
Chromatographic condition and system suitability: take octadecylsilane chemically bonded silica as filling agent; Take methyl alcohol: water=20:80 as mobile phase; The detection wavelength is 270nm; Number of theoretical plate calculates by the gentiamarin peak should be not less than 3000;
The preparation of reference substance solution: it is an amount of to get the gentiamarin reference substance, accurately weighed, adds methyl alcohol and makes the solution that every 1ml contains 25 μ g, and get final product;
The preparation of need testing solution: get this product Longdanxiegan particle under the content uniformity item, porphyrize is got 1g, accurately weighed, put in the tool plug conical flask the accurate methyl alcohol 25ml that adds, close plug, weighed weight, ultrasonic processing 30 minutes, power is 250W, and frequency is 50kHz, lets cool, weighed weight is supplied the weight that subtracts mistake, mixing with methyl alcohol again, filter, get subsequent filtrate, and get final product;
Determination method: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product;
(2) preparation of reference substance solution: precision takes by weighing at 4 hours scutelloside reference substance of 60 ℃ of drying under reduced pressure an amount of, adds methyl alcohol and makes the solution that every 1ml contains 60 μ l, and get final product;
The need testing solution preparation: get this product Longdanxiegan particle under the content uniformity item, fully porphyrize is got 1.5g, accurately weighed, put in the 50ml measuring bottle, add 60% methyl alcohol 45ml, ultrasonic processing, 30 minutes, power 150W, frequency 25KHz lets cool to room temperature, adds 60% methyl alcohol to scale, shake up, filter, discard just filtrate, get subsequent filtrate, and get final product;
According to an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring;
Chromatographic condition and system suitability: be filling agent with octadecylsilane chemically bonded silica; Methyl alcohol: water: phosphoric acid=47:53:0.2 is mobile phase; The detection wavelength is 280nm; Number of theoretical plate is pressed the scutelloside peak and is calculated, and should be not less than 2500;
Determination method: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, injects liquid chromatography liquid, measures, and get final product;
(3) preparation of reference substance solution: it is an amount of to get the Gardenoside reference substance, accurately weighed, adds 50% methyl alcohol and makes the solution that every 1ml contains 30 μ g, and get final product;
The preparation of need testing solution: get this product Longdanxiegan particle under the content uniformity item, fully porphyrize is got 1.5g, accurately weighed, put in the tool plug conical flask the accurate 50% methyl alcohol 50ml that adds, weighed weight, ultrasonic processing 20 minutes, power is 300W, frequency is 50kHz, let cool, weighed weight is supplied the weight that subtracts mistake with 50% methyl alcohol again, shake up, filter; Precision is measured subsequent filtrate 10ml, puts in the 25ml measuring bottle, adds 50% methyl alcohol to scale, shakes up, and filters, and gets subsequent filtrate, and get final product;
According to an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring;
Chromatographic condition and system suitability: take octadecylsilane chemically bonded silica as filling agent; Take acetonitrile: water=11:89 as mobile phase; The detection wavelength is 238nm, and number of theoretical plate calculates by the Gardenoside peak should be not less than 2000;
Determination method is accurate reference substance solution and each 10 μ l of need testing solution of drawing respectively, and the injection liquid chromatography is measured, and be get final product.
Advantage of the present invention is: standard the detection method of Longdanxiegan particle, by setting up the discriminating of monarch drug in a prescription rough gentian and the ministerial drug root of large-flowered skullcap and the assay of assay and cape jasmine, and cooperate the discriminating of original cape jasmine, the more fully composition of detection of drugs and its compatibility, understand its content and stability, also help to illustrate the medical substance basis of medicine.
Embodiment
The Longdanxiegan particle is provided by prescription and explained hereafter in the background technology by JiLin ZiXin Pharmacy Co., Ltd.
(1) discrimination method
(1) get this product Longdanxiegan particle 12g, porphyrize adds methyl alcohol 50ml, adds hot reflux 1 hour, filter, filtrate evaporate to dryness, residue add water 15ml, and heating makes dissolving, let cool, the full normal butyl alcohol that closes of water extracts 2 times, and each 15ml merges n-butanol extracting liquid, the recovered under reduced pressure normal butyl alcohol is to doing, and residue adds methyl alcohol 2ml makes dissolving, is added on the neutral alumina column of having handled well, the neutral alumina that fills 120 orders, 2g, column internal diameter 15mm, with methyl alcohol 20ml wash-out, eluent is concentrated into 2ml, as need testing solution;
Other gets the gentiamarin reference substance, adds methyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution;
According to the test of an appendix VI of Chinese Pharmacopoeia version in 2005 B thin-layered chromatography, draw each 3 μ l of above-mentioned two kinds of solution, put in same silica G F respectively
254On the thin layer plate, with chloroform: methyl alcohol: water=13:6:2, lower floor's solution of placing below 10 ℃ is developping agent, launches, take out, dry, put inspection knowledge under the 254nm ultraviolet lamp, in the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color;
(2) get this product Longdanxiegan particle 12g, add water 30ml, heating makes dissolving, let cool, use extracted by ether 3 times, each 15ml, discard ether solution, the full normal butyl alcohol that closes of water extracts 3 times again, each 15ml, merge normal butyl alcohol liquid, add the equal-volume ammonia solution, shake up, place layering, divide and get supernatant, the recovered under reduced pressure normal butyl alcohol is to doing, residue adds methyl alcohol 1ml makes dissolving, as need testing solution; Other gets the Gardenoside reference substance, adds methyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; Thin-layered chromatography test with reference to an appendix VI of Chinese Pharmacopoeia version in 2005 B, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, take ethyl acetate: acetone: formic acid: water=5:5:1:1 launches as developping agent, takes out, dry, spray is with ethanol solution of sulfuric acid, and is about 10 minutes of 110 ℃ of bakings, clear to the spot colour developing; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color;
(3) get this product Longdanxiegan particle 12g, porphyrize adds methyl alcohol 50ml, add hot reflux 1 hour, and filtered the filtrate evaporate to dryness, residue adds water 15ml, and heating makes dissolving, lets cool, the full normal butyl alcohol that closes of water extracts 2 times, each 15ml merges n-butanol extracting liquid, and the recovered under reduced pressure normal butyl alcohol is to doing, residue adds methyl alcohol 2ml makes dissolving, as need testing solution; Other gets the scutelloside reference substance, adds methyl alcohol and makes the solution that every 1ml contains 5mg, in contrast product solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin-layered chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, take ethyl acetate: butanone: formic acid: water=5:3:1.1:1 is as developping agent, launch, take out, dry, spray is with 5% ferric trichloride ethanolic solution; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color;
(2) content assaying method
(1) according to an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring;
Chromatographic condition and system suitability: take octadecylsilane chemically bonded silica as filling agent; Take methyl alcohol: water=20:80 as mobile phase; The detection wavelength is 270nm; Number of theoretical plate calculates by the gentiamarin peak should be not less than 3000;
The preparation of reference substance solution: it is an amount of to get the gentiamarin reference substance, accurately weighed, adds methyl alcohol and makes the solution that every 1ml contains 25 μ g, and get final product;
The preparation of need testing solution: get this product Longdanxiegan particle under the content uniformity item, porphyrize is got 1g, accurately weighed, put in the tool plug conical flask the accurate methyl alcohol 25ml that adds, close plug, weighed weight, ultrasonic processing 30 minutes, power is 250W, and frequency is 50kHz, lets cool, weighed weight is supplied the weight that subtracts mistake, mixing with methyl alcohol again, filter, get subsequent filtrate, and get final product;
Determination method: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product;
(2) preparation of reference substance solution: precision takes by weighing at 4 hours scutelloside reference substance of 60 ℃ of drying under reduced pressure an amount of, adds methyl alcohol and makes the solution that every 1ml contains 60 μ l, and get final product;
The need testing solution preparation: get this product Longdanxiegan particle under the content uniformity item, fully porphyrize is got 1.5g, accurately weighed, put in the 50ml measuring bottle, add 60% methyl alcohol 45ml, ultrasonic processing, 30 minutes, power 150W, frequency 25KHz lets cool to room temperature, adds 60% methyl alcohol to scale, shake up, filter, discard just filtrate, get subsequent filtrate, and get final product;
According to an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring;
Chromatographic condition and system suitability: be filling agent with octadecylsilane chemically bonded silica; Methyl alcohol: water: phosphoric acid=47:53:0.2 is mobile phase; The detection wavelength is 280nm; Number of theoretical plate is pressed the scutelloside peak and is calculated, and should be not less than 2500;
Determination method: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, injects liquid chromatography liquid, measures, and get final product;
(3) preparation of reference substance solution: it is an amount of to get the Gardenoside reference substance, accurately weighed, adds 50% methyl alcohol and makes the solution that every 1ml contains 30 μ g, and get final product;
The preparation of need testing solution: get this product Longdanxiegan particle under the content uniformity item, fully porphyrize is got 1.5g, accurately weighed, put in the tool plug conical flask the accurate 50% methyl alcohol 50ml that adds, weighed weight, ultrasonic processing 20 minutes, power is 300W, frequency is 50kHz, let cool, weighed weight is supplied the weight that subtracts mistake with 50% methyl alcohol again, shake up, filter; Precision is measured subsequent filtrate 10ml, puts in the 25ml measuring bottle, adds 50% methyl alcohol to scale, shakes up, and filters, and gets subsequent filtrate, and get final product;
According to an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring;
Chromatographic condition and system suitability: take octadecylsilane chemically bonded silica as filling agent; Take acetonitrile: water=11:89 as mobile phase; The detection wavelength is 238nm, and number of theoretical plate calculates by the Gardenoside peak should be not less than 2000;
Determination method is accurate reference substance solution and each 10 μ l of need testing solution of drawing respectively, and the injection liquid chromatography is measured, and be get final product.
Claims (1)
1. the detection method of a Longdanxiegan particle comprises following discrimination method:
(1) get this product Longdanxiegan particle 12g, add water 30ml, heating makes dissolving, let cool, use extracted by ether 3 times, each 15ml, discard ether solution, the full normal butyl alcohol that closes of water extracts 3 times again, each 15ml, merge normal butyl alcohol liquid, add the equal-volume ammonia solution, shake up, place layering, divide and get supernatant, the recovered under reduced pressure normal butyl alcohol is to doing, residue adds methyl alcohol 1ml makes dissolving, as need testing solution; Other gets the Gardenoside reference substance, adds methyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; Thin-layered chromatography test with reference to an appendix VI of Chinese Pharmacopoeia version in 2005 B, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, take ethyl acetate: acetone: formic acid: water=5:5:1:1 launches as developping agent, takes out, dry, spray is with ethanol solution of sulfuric acid, and is about 10 minutes of 110 ℃ of bakings, clear to the spot colour developing; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color;
Characterized by further comprising following discrimination method and content assaying method:
(1) discrimination method
(2) get this product Longdanxiegan particle 12g, porphyrize adds methyl alcohol 50ml, adds hot reflux 1 hour, filter, filtrate evaporate to dryness, residue add water 15ml, and heating makes dissolving, let cool, the full normal butyl alcohol that closes of water extracts 2 times, and each 15ml merges n-butanol extracting liquid, the recovered under reduced pressure normal butyl alcohol is to doing, and residue adds methyl alcohol 2ml makes dissolving, is added on the neutral alumina column of having handled well, the neutral alumina that fills 120 orders, 2g, column internal diameter 15mm, with methyl alcohol 20ml wash-out, eluent is concentrated into 2ml, as need testing solution;
Other gets the gentiamarin reference substance, adds methyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution;
According to the test of an appendix VI of Chinese Pharmacopoeia version in 2005 B thin-layered chromatography, draw each 3 μ l of above-mentioned two kinds of solution, put in same silica G F respectively
254On the thin layer plate, with chloroform: methyl alcohol: water=13:6:2, lower floor's solution of placing below 10 ℃ is developping agent, launches, take out, dry, put inspection knowledge under the 254nm ultraviolet lamp, in the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color;
(3) get this product Longdanxiegan particle 12g, porphyrize adds methyl alcohol 50ml, add hot reflux 1 hour, and filtered the filtrate evaporate to dryness, residue adds water 15ml, and heating makes dissolving, lets cool, the full normal butyl alcohol that closes of water extracts 2 times, each 15ml merges n-butanol extracting liquid, and the recovered under reduced pressure normal butyl alcohol is to doing, residue adds methyl alcohol 2ml makes dissolving, as need testing solution; Other gets the scutelloside reference substance, adds methyl alcohol and makes the solution that every 1ml contains 5mg, in contrast product solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin-layered chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, take ethyl acetate: butanone: formic acid: water=5:3:1.1:1 is as developping agent, launch, take out, dry, spray is with 5% ferric trichloride ethanolic solution; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color;
(2) content assaying method
(1) according to an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring;
Chromatographic condition and system suitability: take octadecylsilane chemically bonded silica as filling agent; Take methyl alcohol: water=20:80 as mobile phase; The detection wavelength is 270nm; Number of theoretical plate calculates by the gentiamarin peak should be not less than 3000;
The preparation of reference substance solution: it is an amount of to get the gentiamarin reference substance, accurately weighed, adds methyl alcohol and makes the solution that every 1ml contains 25 μ g, and get final product;
The preparation of need testing solution: get this product Longdanxiegan particle under the content uniformity item, porphyrize is got 1g, accurately weighed, put in the tool plug conical flask the accurate methyl alcohol 25ml that adds, close plug, weighed weight, ultrasonic processing 30 minutes, power is 250W, and frequency is 50kHz, lets cool, weighed weight is supplied the weight that subtracts mistake, mixing with methyl alcohol again, filter, get subsequent filtrate, and get final product;
Determination method: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product;
(2) preparation of reference substance solution: precision takes by weighing at 4 hours scutelloside reference substance of 60 ℃ of drying under reduced pressure an amount of, adds methyl alcohol and makes the solution that every 1ml contains 60 μ l, and get final product;
The need testing solution preparation: get this product Longdanxiegan particle under the content uniformity item, fully porphyrize is got 1.5g, accurately weighed, put in the 50ml measuring bottle, add 60% methyl alcohol 45ml, ultrasonic processing, 30 minutes, power 150W, frequency 25KHz lets cool to room temperature, adds 60% methyl alcohol to scale, shake up, filter, discard just filtrate, get subsequent filtrate, and get final product;
According to an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring;
Chromatographic condition and system suitability: be filling agent with octadecylsilane chemically bonded silica; Methyl alcohol: water: phosphoric acid=47:53:0.2 is mobile phase; The detection wavelength is 280nm; Number of theoretical plate is pressed the scutelloside peak and is calculated, and should be not less than 2500;
Determination method: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, injects liquid chromatography liquid, measures, and get final product;
(3) preparation of reference substance solution: it is an amount of to get the Gardenoside reference substance, accurately weighed, adds 50% methyl alcohol and makes the solution that every 1ml contains 30 μ g, and get final product;
The preparation of need testing solution: get this product Longdanxiegan particle under the content uniformity item, fully porphyrize is got 1.5g, accurately weighed, put in the tool plug conical flask the accurate 50% methyl alcohol 50ml that adds, weighed weight, ultrasonic processing 20 minutes, power is 300W, frequency is 50kHz, let cool, weighed weight is supplied the weight that subtracts mistake with 50% methyl alcohol again, shake up, filter; Precision is measured subsequent filtrate 10ml, puts in the 25ml measuring bottle, adds 50% methyl alcohol to scale, shakes up, and filters, and gets subsequent filtrate, and get final product;
According to an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring;
Chromatographic condition and system suitability: take octadecylsilane chemically bonded silica as filling agent; Take acetonitrile: water=11:89 as mobile phase; The detection wavelength is 238nm, and number of theoretical plate calculates by the Gardenoside peak should be not less than 2000;
Determination method is accurate reference substance solution and each 10 μ l of need testing solution of drawing respectively, and the injection liquid chromatography is measured, and be get final product.
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Application publication date: 20130424 |