CN102091168A - Quality control method for Chinese medicine preparation Xuefuzhuyu capsule - Google Patents
Quality control method for Chinese medicine preparation Xuefuzhuyu capsule Download PDFInfo
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Abstract
The invention belongs to the technical field of Chinese patent medicines, and relates to a quality control method for a Chinese medicine preparation Xuefuzhuyu capsule prepared from traditional Chinese medicinal materials. In the quality control method, citrus trifoliata is utilized as a comparison medicinal material, naringin is used as a comparison product, Chinese angelica and szechwan lovage rhizome are used as comparison medicinal materials, Chinese thorowax root is used as a comparison medicinal material, liquorice is used as a comparison medicinal material, and whether the formula of the Xuefuzhuyu capsule contains citrus trifoliata, Chinese angelica szechwan lovage rhizome, Chinese thorowax root and liquorice is identified by means of thin-layer chromatography; and amygdalin is used as a comparison product, and whether peach seed is contained in the Xuefuzhuyu capsule is identified by means of high performance liquid chromatography. By utilizing the quality control method provided by the invention, fraudulent medicaments and inferior medicaments can be identified more accurately, so as to improve the safety in use. By utilizing an inspection method for determining the content of paeoniflorin used as a quantitative indicator by means of high performance liquid chromatography, the controllability of the quality standards of the Xuefuzhuyu capsule is improved, and the inherent quality and curative effect of products are further ensured; and the revised quality standards are improved, and the quality control of the Xuefuzhuyu capsule is improved.
Description
Technical field
The invention belongs to the technical field of Chinese patent medicine, relating to the Chinese crude drug is the method for quality control of a kind of Chinese medicine preparation XUEFU ZHUYU JIAONANG of making of raw material.
Background technology
XUEFU ZHUYU JIAONANG is a kind of classical Chinese patent medicine, is " the Sanitation Ministry medicine standard " the 16 51 pages of preparations that record, Ministry of Public Health standard WS
3-B-3049-98 record prescription and quality standard:
Prescription:
Semen Persicae (stir-fry) Radix Angelicae Sinensis Fructus Aurantii (parched with bran) Rhizoma Chuanxiong
Radix Bupleuri Flos Carthami Radix Achyranthis Bidentatae Radix Paeoniae Rubra
Radix Rehmanniae Radix Platycodonis Radix Glycyrrhizae
Method for making: get ten Herba indigoferae Pseudotinctoriae water extraction 1-3 times such as Radix Angelicae Sinensis, water consumption 6-10 doubly, each 0.5-1.5h, filter, collect filtrate, being evaporated to relative density is 1.07-1.35 (60-70 ℃), treats cold placement room temperature, adds ethanol and makes and contain the alcohol amount and be 60-80%, stir evenly, leave standstill (5-25h) and make precipitation, get supernatant and be evaporated to the starch that relative density is 1.30-1.50 (60-70 ℃) adding extractum amount 10-15%, dry 5-12h in drying baker (T=65-80 ℃), get dry thing (dried cream rate 20-28%), add the silicon dioxide of dry thing weight 2%-8%, incapsulate, pulverized the 24-60 mesh sieve.(every gram capsule is equivalent to crude drug 3.10 ~ 3.38g)
Semen Persicae (stir-fry), Radix Angelicae Sinensis, Radix Bupleuri, Rhizoma Chuanxiong, Fructus Aurantii (parched with bran) in the microscopical identification prescription are set in the standard; Thin layer chromatography differentiates in the prescription whether contain Fructus Aurantii (hesperidin), Radix Paeoniae Rubra composition; High performance liquid chromatography (appendix VI D) is measured content of paeoniflorin in the prescription
Similar to XUEFU ZHUYU JIAONANG standard record prescription at present, the similar product document of effect is a lot, but do not see that the record prescription is identical, the product document that effect is identical, but in the existing XUEFU ZHUYU JIAONANG method of quality control that Ministry of Public Health is issued, differentiating under the item that microscopical identification is only arranged, the thin layer of Fructus Aurantii medical material is differentiated, only a kind of composition of peoniflorin is carried out quantitatively under the assay item.For by the ten compound recipe XUEFU ZHUYU JIAONANG formed of medical material simply, only with the assay of the qualitative identification of medical material simply and single index composition as its method of quality control, specificity is not strong, limitation is bigger, can not reflect product quality homogeneity and stability comprehensively, be difficult to control the quality of XUEFU ZHUYU JIAONANG.For improving the product quality of Chinese medicine, need improve target level of product quality.
Summary of the invention
The objective of the invention is to the objective of the invention is to overcome the XUEFU ZHUYU JIAONANG standard weak point of prior art, a kind of method of quality control of XUEFU ZHUYU JIAONANG of qualitative and quantitative analysis ingredient that can be more perfect is provided.
In order to reach the technical scheme that purpose of the present invention adopts be: a kind of method of quality control of Chinese medicine preparation XUEFU ZHUYU JIAONANG, wherein said pharmaceutical formulation are by Chinese crude drug:
Radix Bupleuri 27g Radix Angelicae Sinensis 81g Radix Rehmanniae 81g Radix Paeoniae Rubra 54g Flos Carthami 81g
Semen Persicae (stir-fry) 108g Fructus Aurantii (parched) 54g Radix Glycyrrhizae 27g Rhizoma Chuanxiong 40.5g
Radix Achyranthis Bidentatae 81g Radix Platycodonis 40.5g forms,
Method for making: above ten simply, and part Semen Persicae (stir-fry), Radix Angelicae Sinensis, Radix Paeoniae Rubra, Fructus Aurantii, Rhizoma Chuanxiong, Radix Bupleuri are ground into fine powder, sieve, mixing, the five tastes such as all the other Flos Carthamis and part Semen Persicae (stir-fry) decoct with water three times, filter, merging filtrate is condensed into thick paste, with above-mentioned powder mixing, make granule, oven dry is pulverized, sieve, incapsulate, make 1000, that is, it is characterized in that: the step of its method is:
(1) with the Fructus Aurantii is control medicinal material, be reference substance with the naringin, be control medicinal material with Radix Angelicae Sinensis, Rhizoma Chuanxiong, with Radix Bupleuri is control medicinal material, is control medicinal material with the Radix Glycyrrhizae, and thin layer chromatography differentiates in the XUEFU ZHUYU JIAONANG prescription whether contain Fructus Aurantii, Radix Angelicae Sinensis, Rhizoma Chuanxiong, Radix Bupleuri, licorice ingredient; With the amygdaloside is reference substance, and high performance liquid chromatography differentiates in the XUEFU ZHUYU JIAONANG prescription whether contain the Semen Persicae composition;
(2) with the peoniflorin be reference substance, high performance liquid chromatography detects content of paeoniflorin in the XUEFU ZHUYU JIAONANG prescription.
The method of quality control of described Chinese medicine preparation XUEFU ZHUYU JIAONANG, it is characterized in that: described thin layer chromatography differentiates that the method that whether contains the Fructus Aurantii composition in the XUEFU ZHUYU JIAONANG prescription is: get this product 5g, add methanol 20ml, supersound extraction 1 hour, left standstill 2 hours, filter, filtrate is concentrated into 10ml, as need testing solution.Other gets Fructus Aurantii control medicinal material 1g, adds methanol 10ml, and supersound extraction 30 minutes filters, in contrast medical material solution; Get the naringin reference substance again, add methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer chromatography (appendix VIB), drawing each 6-8 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, is developing solvent with the ethyl acetate, alcohol and water, ethyl acetate: ethanol: water=8: 2: 1, launch, take out, dry, spray is with the aluminum chloride test solution, put and inspect under the ultra-violet lamp 365nm in the test sample chromatograph, with control medicinal material, the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
Described thin layer chromatography differentiates that the method that whether contains Radix Angelicae Sinensis, Rhizoma Chuanxiong composition in the XUEFU ZHUYU JIAONANG prescription is: get this product powder 3g, add petroleum ether (60 ℃-90 ℃) 10ml, supersound process 10 minutes filters, and filtrate is as need testing solution.Other gets Radix Angelicae Sinensis control medicinal material powder 1g, adds petroleum ether (60 ℃-90 ℃) 10ml, and supersound process 10 minutes filters, and filtrate is medical material solution in contrast.Get Rhizoma Chuanxiong control medicinal material powder 1g again, add petroleum ether (60 ℃-90 ℃) 10ml, supersound process 10 minutes filters, and filtrate is medical material solution in contrast; 2-5 μ l is drawn in thin layer chromatography (appendix VIB of Chinese Pharmacopoeia) test, puts respectively on same silica gel g thin-layer plate, and be developing solvent with normal hexane-ethyl acetate, normal hexane: ethyl acetate=9: 1, launch, take out, dry, put ultra-violet lamp 365nm, inspect down; In the test sample chromatograph chromatograph, with the corresponding position of control medicinal material chromatograph on, show the sapphirine fluorescence speckle of same color;
Described thin layer chromatography differentiates that the method that whether contains the Radix Bupleuri composition in the XUEFU ZHUYU JIAONANG prescription is: get this product powder 4.0g, add methanol 30ml, supersound process 30min, put coldly, filter the filtrate evaporate to dryness, residue adds water 30ml makes dissolving, extracts 3 times with the water-saturated n-butanol jolting, each 20ml, merge n-butyl alcohol liquid, with ammonia solution 50ml washing 1 time, the water 50ml that the reuse n-butyl alcohol is saturated washs the n-butyl alcohol evaporate to dryness 1 time, residue adds methanol 2ml makes dissolving, as need testing solution.Other gets Radix Bupleuri control medicinal material 0.5g, adds methanol 30ml, supersound process 30min, put coldly, filter the filtrate evaporate to dryness, residue adds water 30ml makes dissolving, extracts 3 times with the water-saturated n-butanol jolting, each 20ml, merge n-butyl alcohol liquid, with ammonia solution 50ml washing 1 time, the water 50ml that the reuse n-butyl alcohol is saturated washs the n-butyl alcohol evaporate to dryness 1 time, residue adds methanol 2ml makes dissolving, in contrast medical material solution.According to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia B) test, draw solution 5 μ l put respectively on same silica gel g thin-layer plate, with chloroform-methanol-water is developing solvent, chloroform: methanol: water=13: 7: 2 lower floor's solution, launch, take out, dry, spray is with 40% sulfuric acid solution of 2% paradime thylaminobenzaldehyde, and 105 ℃ of heating colour developings are in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color; Put under the ultra-violet lamp 365nm and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
Described thin layer chromatography differentiates that the method that whether contains licorice ingredient in the XUEFU ZHUYU JIAONANG prescription is: get this product powder 4.0g, add methanol 40ml, supersound process 30min filters, the filtrate evaporate to dryness, residue adds water 20ml makes dissolving, extracts 2 times with the ether jolting, each 20ml, discard ether solution, the jolting of reuse water-saturated n-butanol is extracted 2 times, and each 20ml merges n-butyl alcohol liquid; With the saturated water washing of n-butyl alcohol 2 times, each 20ml; Discard water liquid, n-butyl alcohol liquid evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution; Extracting liquorice control medicinal material 0.5g adds methanol 40ml in addition, and supersound process 30min filters, filtrate evaporate to dryness, residue add water 20ml makes dissolving, extracts 2 times with the ether jolting, each 20ml, discard ether solution, the jolting of reuse water-saturated n-butanol is extracted 2 times, and each 20ml merges n-butyl alcohol liquid; With the saturated water washing of n-butyl alcohol 2 times, each 20ml; Discard water liquid, n-butyl alcohol liquid evaporate to dryness, residue add methanol 2ml makes dissolving, in contrast medical material solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia B), draw solution 10 μ l put respectively on same silica gel g thin-layer plate, are developing solvent with chloroform-methanol-water, chloroform: methanol: water=13: 6: 2 lower floor's solution, launch, take out, dry, spray is with 105 ℃ of heating colour developings of 10% sulphuric acid ethanol, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color; Put under the 365nm and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
Described is reference substance with the amygdaloside, and high performance liquid chromatography differentiates that the method that whether contains the Semen Persicae composition in the XUEFU ZHUYU JIAONANG prescription is:
(1) chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; With methanol is mobile phase A, is Mobile phase B with water, and the regulation in the according to the form below 1 is carried out gradient elution; The detection wavelength is 210nm;
(2) preparation of reference substance solution: get the amygdaloside reference substance, add methanol and make the solution that every 1ml contains 60 μ g, in contrast product solution;
(3) preparation of need testing solution: get this product content under the content uniformity item, mixing is got 0.5g, the accurate title, decide, and puts in the tool plug conical flask, the accurate 50% methanol 25ml that adds, supersound process (power 250w, frequency 50kHz) 30 minutes is put cold, claim to decide weight again, supply the weight that subtracts mistake with 50% methanol, shake up, filter, get subsequent filtrate, promptly;
(4) algoscopy: draw each 20 μ l of reference substance solution and need testing solution respectively, inject chromatograph of liquid.Test sample should present the chromatographic peak identical with the reference substance retention time.
Table 1 gradient elution table
The method of quality control of described Chinese medicine preparation XUEFU ZHUYU JIAONANG is characterized in that: be reference substance with the peoniflorin, the method that high performance liquid chromatography detects content of paeoniflorin in the XUEFU ZHUYU JIAONANG prescription is:
(1) chromatographic condition and system suitability test: with the octadecylsilane bonded silica is filler; With acetonitrile-water-glacial acetic acid (16: 84: 1) is mobile phase; The detection wavelength is 230nm.Number of theoretical plate calculates by peoniflorin should be not less than 2500;
(2) preparation of reference substance solution: it is an amount of to get the peoniflorin reference substance, and accurate the title decides, and adds 50% methanol and makes the solution that contains peoniflorin 0.2mg among every 1ml, promptly;
(3) preparation of need testing solution: get this product content under the content uniformity item, mixing is got 0.5g, the accurate title, decide, and puts in the tool plug conical flask, the accurate 50% methanol 25ml that adds, supersound process (power 250w, frequency 50kHz) 30 minutes is put cold, claim to decide weight again, supply the weight that subtracts mistake with 50% methanol, shake up, filter, get subsequent filtrate, promptly
(4) algoscopy: accurate respectively reference substance solution and each 20ul of need testing solution of drawing, inject chromatograph of liquid, measure, promptly; Every of this product contains Radix Paeoniae Rubra with peoniflorin (C
23H
28O
11) meter, must not be less than 1.0mg.
The invention beneficial effect: being provided with the Fructus Aurantii in the quality standard is control medicinal material, be reference substance with the naringin, be control medicinal material with Radix Angelicae Sinensis, Rhizoma Chuanxiong, with Radix Bupleuri is control medicinal material, with the Radix Glycyrrhizae is control medicinal material, and thin layer chromatography differentiates in the XUEFU ZHUYU JIAONANG prescription whether contain Fructus Aurantii, Radix Angelicae Sinensis, Rhizoma Chuanxiong, Radix Bupleuri, licorice ingredient; With the amygdaloside is reference substance, and high performance liquid chromatography differentiates in the XUEFU ZHUYU JIAONANG prescription whether contain the Semen Persicae composition; Can check out counterfeit drug and substandard drug more exactly, improve the safety in using; High performance liquid chromatography detects content of paeoniflorin in the XUEFU ZHUYU JIAONANG prescription, determines that every contains Radix Paeoniae Rubra with peoniflorin (C
23H
28O
11) count, must not be less than the quantitative target and the method for inspection of 1.0mg, improved the controllability of XUEFU ZHUYU JIAONANG quality standard, further guarantee product inherent quality and curative effect, make quality standard comparatively perfect, revised quality standard has improved the quality control of medicine.
The specific embodiment
Below in conjunction with embodiment, the present invention is further described, the XUEFU ZHUYU JIAONANG quality standard after embodiment 1 improves:
Prescription:
Radix Bupleuri 27g Radix Angelicae Sinensis 81g Radix Rehmanniae 81g Radix Paeoniae Rubra 54g Flos Carthami 81g
Semen Persicae (stir-fry) 108g Fructus Aurantii (parched) 54g Radix Glycyrrhizae 27g Rhizoma Chuanxiong 40.5g
Radix Achyranthis Bidentatae 81g Radix Platycodonis 40.5g
Method for making: above ten simply, and part Semen Persicae (stir-fry), Radix Angelicae Sinensis, Radix Paeoniae Rubra, Fructus Aurantii, Rhizoma Chuanxiong, Radix Bupleuri are ground into fine powder, sieve, mixing, the five tastes such as all the other Flos Carthamis and part Semen Persicae (stir-fry) decoct with water three times, filter, merging filtrate is condensed into thick paste, with above-mentioned powder mixing, make granule, oven dry is pulverized, sieve, incapsulate, make 1000, promptly.
Character: this product is a capsule, and content is tan powder; The gas suffering, mildly bitter flavor.
Differentiate: (1) gets this product, and put microscopically and observe: thin-layer cell spindle, wall are slightly thick, and atomic thin oblique cross lamination is arranged.Oil pipe contains yellow or brown secretions.Spiral duct footpath 8～23 μ m, thickened wall is interconnection, and like netted spiral duct, prism of calcium oxalate is present in the parenchyma in flakes.
(2) get this product 5g, add methanol 20ml, supersound extraction 1 hour left standstill 2 hours, filtered, and filtrate is concentrated into 10ml, as need testing solution.Other gets Fructus Aurantii control medicinal material 1g, adds methanol 10ml, and supersound extraction 30 minutes filters, in contrast medical material solution.Get the naringin reference substance again, add methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution.According to thin layer chromatography (appendix VIB) test, draw each 6-8 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate, alcohol and water (8: 2: 1) is developing solvent, launches, and takes out, dry, spray is put under the ultra-violet lamp (365nm) and is inspected with the aluminum chloride test solution.In the test sample chromatograph, with control medicinal material, the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
(3) get this product powder 3g, add petroleum ether (60 ℃-90 ℃) 10ml, supersound process 10 minutes filters, and filtrate is as need testing solution.Other gets Radix Angelicae Sinensis control medicinal material powder 1g, adds petroleum ether (60 ℃-90 ℃) 10ml, and supersound process 10 minutes filters, and filtrate is medical material solution in contrast.Get Rhizoma Chuanxiong control medicinal material powder 1g again, add petroleum ether (60 ℃-90 ℃) 10ml, supersound process 10 minutes filters, and filtrate is medical material solution in contrast.2-5 μ l is drawn in thin layer chromatography (appendix VIB) test, puts respectively on same silica gel g thin-layer plate, and be developing solvent with normal hexane-ethyl acetate (9: 1), launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph chromatograph, with the corresponding position of control medicinal material chromatograph on, show the sapphirine fluorescence speckle of same color.
(4) get this product powder 4.0g, add methanol 30ml, supersound process 30min, put coldly, filter the filtrate evaporate to dryness, residue adds water 30ml makes dissolving, extracts 3 times with the water-saturated n-butanol jolting, each 20ml, merge n-butyl alcohol liquid, with ammonia solution 50ml washing 1 time, the water 50ml that the reuse n-butyl alcohol is saturated washs the n-butyl alcohol evaporate to dryness 1 time, residue adds methanol 2ml makes dissolving, as need testing solution.Other gets Radix Bupleuri control medicinal material 0.5g, adds methanol 30ml, supersound process 30min, put coldly, filter the filtrate evaporate to dryness, residue adds water 30ml makes dissolving, extracts 3 times with the water-saturated n-butanol jolting, each 20ml, merge n-butyl alcohol liquid, with ammonia solution 50ml washing 1 time, the water 50ml that the reuse n-butyl alcohol is saturated washs the n-butyl alcohol evaporate to dryness 1 time, residue adds methanol 2ml makes dissolving, in contrast medical material solution.Test according to thin layer chromatography (appendix VI B), draw solution 5 μ l put respectively on same silica gel g thin-layer plate, and lower floor is developing solvent with chloroform-methanol-water (13: 7: 2), launch, take out, dry, spray is with 40% sulfuric acid solution of 2% paradime thylaminobenzaldehyde, 105 ℃ of heating colour developings, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color; Put under the ultra-violet lamp 365nm and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color
(5) get this product powder 4.0g, add methanol 40ml, supersound process 30min filters, filtrate evaporate to dryness, residue add water 20ml makes dissolving, extracts 2 times with the ether jolting, each 20ml, discard ether solution, the jolting of reuse water-saturated n-butanol is extracted 2 times, and each 20ml merges n-butyl alcohol liquid; With the saturated water washing of n-butyl alcohol 2 times, each 20ml; Discard water liquid, n-butyl alcohol liquid evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution.Extracting liquorice control medicinal material 0.5g adds methanol 40ml in addition, and supersound process 30min filters, filtrate evaporate to dryness, residue add water 20ml makes dissolving, extracts 2 times with the ether jolting, each 20ml, discard ether solution, the jolting of reuse water-saturated n-butanol is extracted 2 times, and each 20ml merges n-butyl alcohol liquid; With the saturated water washing of n-butyl alcohol 2 times, each 20ml; Discard water liquid, n-butyl alcohol liquid evaporate to dryness, residue add methanol 2ml makes dissolving, in contrast medical material solution.Test according to thin layer chromatography (appendix VI B), draw solution 10 μ l, putting respectively on same silica gel g thin-layer plate, is developing solvent with chloroform-methanol-water (13: 6: 2) lower floor solution, launches, take out, dry, spray is with 105 ℃ of heating colour developings of 10% sulphuric acid ethanol, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color; Put under the 365nm and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(6) need testing solution of getting under the assay item is a need testing solution.Other gets the amygdaloside reference substance, adds methanol and makes the solution that every 1ml contains 60 μ g, in contrast product solution.According to high performance liquid chromatography (appendix VI D) test, be filler with octadecylsilane chemically bonded silica; With methanol is mobile phase A, is Mobile phase B with water, and the regulation in the according to the form below is carried out gradient elution; The detection wavelength is 210nm.Draw each 20 μ l of reference substance solution and need testing solution respectively, inject chromatograph of liquid.Test sample should present the chromatographic peak identical with the reference substance retention time.
Check: should meet every regulation relevant under the capsule item (appendix IA).
Assay: measure according to high performance liquid chromatography (appendix VI D).
Chromatographic condition and employment and suitability test (E ﹠ ST): with the octadecylsilane bonded silica is filler; With acetonitrile-water-glacial acetic acid (16: 84: 1) is mobile phase; The detection wavelength is 230nm.Number of theoretical plate calculates by peoniflorin should be not less than 2500.
The preparation of reference substance solution: it is an amount of to get the peoniflorin reference substance, and accurate the title decides, and adds 50% methanol and makes the solution that contains peoniflorin 0.2mg among every 1ml, promptly.
The preparation of need testing solution: get this product content under the content uniformity item, mixing is got 0.5g, the accurate title, decide, and puts in the tool plug conical flask, the accurate 50% methanol 25ml that adds, supersound process (power 250w, frequency 50kHz) 30 minutes is put cold, claim to decide weight again, supply the weight that subtracts mistake with 50% methanol, shake up, filter, get subsequent filtrate, promptly.
Algoscopy: accurate respectively reference substance solution and each 20ul of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.
Every of this product contains Radix Paeoniae Rubra with peoniflorin (C
23H
28O
11) meter, must not be less than 1.0mg.Function with cure mainly: blood circulation promoting and blood stasis dispelling, promoting the circulation of QI to relieve pain.Be used for blood-stasis internal-depression, chest pain or headache, interior-heat blurring of vision accompanied with oppressive feeling, insomnia and dreamful sleep, severe palpitation, impatience and irascibility; Angina pectoris, blood vessel and traumatic headache belong to above-mentioned disease person.
Usage and consumption: oral, one time 6,2 times on the one, one month is a course of treatment.
Specification: every dress 0.4g
Storage: sealing, put shady and cool dry place.
Claims (3)
1. the method for quality control of a Chinese medicine preparation XUEFU ZHUYU JIAONANG, wherein said pharmaceutical formulation are by Chinese crude drug:
Radix Bupleuri 27g Radix Angelicae Sinensis 81g Radix Rehmanniae 81g Radix Paeoniae Rubra 54g Flos Carthami 81g Semen Persicae (parched) 108g Fructus Aurantii (parched) 54g Radix Glycyrrhizae 27g Rhizoma Chuanxiong 40.5g Radix Achyranthis Bidentatae 81g Radix Platycodonis 40.5g forms, method for making: above ten simply, the part Semen Persicae (parched), Radix Angelicae Sinensis, Radix Paeoniae Rubra, Fructus Aurantii (parched), Rhizoma Chuanxiong, Radix Bupleuri is ground into fine powder, sieve, mixing, the five tastes such as all the other Flos Carthamis and part Semen Persicae (parched) decoct with water three times, filter, merging filtrate is condensed into thick paste, with above-mentioned powder mixing, make granule, oven dry is pulverized, and sieves, incapsulate, make 1000, that is, it is characterized in that: the step of its method is:
(1) with the Fructus Aurantii is control medicinal material, be reference substance with the naringin, be control medicinal material with Radix Angelicae Sinensis, Rhizoma Chuanxiong, with Radix Bupleuri is control medicinal material, is control medicinal material with the Radix Glycyrrhizae, and thin layer chromatography differentiates in the XUEFU ZHUYU JIAONANG prescription whether contain Fructus Aurantii, Radix Angelicae Sinensis, Rhizoma Chuanxiong, Radix Bupleuri, licorice ingredient; With the amygdaloside is reference substance, and high performance liquid chromatography differentiates in the XUEFU ZHUYU JIAONANG prescription whether contain the Semen Persicae composition;
(2) with the peoniflorin be reference substance, high performance liquid chromatography detects content of paeoniflorin in the XUEFU ZHUYU JIAONANG prescription.
2. the method for quality control of Chinese medicine preparation XUEFU ZHUYU JIAONANG according to claim 1 is characterized in that:
Described thin layer chromatography differentiates that the method that whether contains the Fructus Aurantii composition in the XUEFU ZHUYU JIAONANG prescription is: get this product 5g, add methanol 20ml, supersound extraction 1 hour left standstill 2 hours, filtered, and filtrate is concentrated into 10ml, as need testing solution; Other gets Fructus Aurantii control medicinal material 1g, adds methanol 10ml, and supersound extraction 30 minutes filters, in contrast medical material solution; Get the naringin reference substance again, add methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer chromatography, drawing each 6-8 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, is developing solvent with the ethyl acetate, alcohol and water, ethyl acetate: ethanol: water=8: 2: 1, launch, take out, dry, spray is with the aluminum chloride test solution, put and inspect under the ultra-violet lamp 365nm in the test sample chromatograph, with control medicinal material, the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
Described thin layer chromatography differentiates that the method that whether contains Radix Angelicae Sinensis, Rhizoma Chuanxiong composition in the XUEFU ZHUYU JIAONANG prescription is: get this product powder 3g, add 60 ℃ of-90 ℃ of petroleum ether 10ml, supersound process 10 minutes filters, and filtrate is as need testing solution.Other gets Radix Angelicae Sinensis control medicinal material powder 1g, adds 60 ℃ of-90 ℃ of petroleum ether 10ml, and supersound process 10 minutes filters, and filtrate is medical material solution in contrast; Get Rhizoma Chuanxiong control medicinal material powder 1g again, add 60 ℃ of-90 ℃ of petroleum ether 10ml, supersound process 10 minutes filters, and filtrate is medical material solution in contrast; 2-5 μ l is drawn in the thin layer chromatography test, puts respectively on same silica gel g thin-layer plate, and be developing solvent with normal hexane-ethyl acetate, normal hexane: ethyl acetate=9: 1, launch, take out, dry, put ultra-violet lamp 365nm, inspect down; In the test sample chromatograph chromatograph, with the corresponding position of control medicinal material chromatograph on, show the sapphirine fluorescence speckle of same color;
Described thin layer chromatography differentiates that the method that whether contains the Radix Bupleuri composition in the XUEFU ZHUYU JIAONANG prescription is: get this product powder 4.0g, add methanol 30ml, supersound process 30min, put coldly, filter the filtrate evaporate to dryness, residue adds water 30ml makes dissolving, extracts 3 times with the water-saturated n-butanol jolting, each 20ml, merge n-butyl alcohol liquid, with ammonia solution 50ml washing 1 time, the water 50ml that the reuse n-butyl alcohol is saturated washs the n-butyl alcohol evaporate to dryness 1 time, residue adds methanol 2ml makes dissolving, as need testing solution; Other gets Radix Bupleuri control medicinal material 0.5g, adds methanol 30ml, supersound process 30min, put coldly, filter the filtrate evaporate to dryness, residue adds water 30ml makes dissolving, extracts 3 times with the water-saturated n-butanol jolting, each 20ml, merge n-butyl alcohol liquid, with ammonia solution 50ml washing 1 time, the water 50ml that the reuse n-butyl alcohol is saturated washs the n-butyl alcohol evaporate to dryness 1 time, residue adds methanol 2ml makes dissolving, in contrast medical material solution; According to the thin layer chromatography test, draw solution 5 μ l put respectively on same silica gel g thin-layer plate, with chloroform-methanol-water is developing solvent, chloroform: methanol: water=13: 7: 2 lower floor's solution, launch, take out, dry, spray is with 40% sulfuric acid solution of 2% paradime thylaminobenzaldehyde, and 105 ℃ of heating colour developings are in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color; Put under the ultra-violet lamp 365nm and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
Described thin layer chromatography differentiates that the method that whether contains licorice ingredient in the XUEFU ZHUYU JIAONANG prescription is: get this product powder 4.0g, add methanol 40ml, supersound process 30min filters, the filtrate evaporate to dryness, residue adds water 20ml makes dissolving, extracts 2 times with the ether jolting, each 20ml, discard ether solution, the jolting of reuse water-saturated n-butanol is extracted 2 times, and each 20ml merges n-butyl alcohol liquid; With the saturated water washing of n-butyl alcohol 2 times, each 20ml; Discard water liquid, n-butyl alcohol liquid evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution; Extracting liquorice control medicinal material 0.5g adds methanol 40ml in addition, and supersound process 30min filters, filtrate evaporate to dryness, residue add water 20ml makes dissolving, extracts 2 times with the ether jolting, each 20ml, discard ether solution, the jolting of reuse water-saturated n-butanol is extracted 2 times, and each 20ml merges n-butyl alcohol liquid; With the saturated water washing of n-butyl alcohol 2 times, each 20ml; Discard water liquid, n-butyl alcohol liquid evaporate to dryness, residue add methanol 2ml makes dissolving, in contrast medical material solution; Test according to thin layer chromatography, draw solution 10 μ l put respectively on same silica gel g thin-layer plate, are developing solvent with chloroform-methanol-water, chloroform: methanol: water=13: 6: 2 lower floor's solution, launch, take out, dry, spray is with 105 ℃ of heating colour developings of 10% sulphuric acid ethanol, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color; Put under the 365nm and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
Described is reference substance with the amygdaloside, and high performance liquid chromatography differentiates that the method that whether contains the Semen Persicae composition in the XUEFU ZHUYU JIAONANG prescription is:
(1) chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; With methanol is mobile phase A, is Mobile phase B with water, and the regulation in the according to the form below 1 is carried out gradient elution; The detection wavelength is 210nm;
(2) preparation of reference substance solution: get the amygdaloside reference substance, add methanol and make the solution that every 1ml contains 60 μ g, in contrast product solution;
(3) preparation of need testing solution: get this product content under the content uniformity item, mixing is got 0.5g, the accurate title, decide, and puts in the tool plug conical flask, the accurate 50% methanol 25ml that adds, supersound process (power 250w, frequency 50kHz) 30 minutes is put cold, claim to decide weight again, supply the weight that subtracts mistake with 50% methanol, shake up, filter, get subsequent filtrate, promptly;
(4) algoscopy: draw each 20 μ l of reference substance solution and need testing solution respectively, inject chromatograph of liquid.Test sample should present the chromatographic peak identical with the reference substance retention time.
Table 1 gradient elution table
3. the method for quality control of Chinese medicine preparation XUEFU ZHUYU JIAONANG according to claim 1 is characterized in that: be reference substance with the peoniflorin, the method that high performance liquid chromatography detects content of paeoniflorin in the XUEFU ZHUYU JIAONANG prescription is:
(1) chromatographic condition and system suitability test: with the octadecylsilane bonded silica is filler; With acetonitrile: water: glacial acetic acid=16: 84: 1 is a mobile phase; The detection wavelength is 230nm; Number of theoretical plate calculates by peoniflorin should be not less than 2500;
(2) preparation of reference substance solution: it is an amount of to get the peoniflorin reference substance, and accurate the title decides, and adds 50% methanol and makes the solution that contains peoniflorin 0.2mg among every 1ml, promptly;
(3) preparation of need testing solution: get this product content under the content uniformity item, mixing is got 0.5g, the accurate title, decide, and puts in the tool plug conical flask, the accurate 50% methanol 25ml that adds, supersound process power 250w frequency 50kHz30 minute, is put cold, claim to decide weight again, supply the weight that subtracts mistake with 50% methanol, shake up, filter, get subsequent filtrate, promptly
(4) algoscopy: accurate respectively reference substance solution and each 20ul of need testing solution of drawing, inject chromatograph of liquid, measure, promptly; Every of this product contains Radix Paeoniae Rubra with peoniflorin (C
23H
28O
11) meter, must not be less than 1.0mg.
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