CN102091167A - Quality control method for Xuefuzhuyu capsule - Google Patents
Quality control method for 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 Xuefuzhuyu capsule prepared from traditional Chinese medicinal materials. In the quality control method, Chinese thorowax root and licorice root are utilized as comparison medicinal materials, and whether the formula of the Xuefuzhuyu capsule contains Chinese thorowax root and licorice root components is identified by means of thin-layer chromatography; and amygdalin (c20h27no11), paeoniflorin (c23h28o11) and naringin (c27h32o14) are used as comparison products, and the contents of the amygdalin, paeoniflorin and naringin in the formula of the Xuefuzhuyu capsule are determined by means of high performance liquid chromatography. By utilizing the quality control method provided by the invention, the situation in the original standards that the quality of compound prescription is controlled by controlling the content of a single indicator component is changed, and the controllability of the quality standards of the Xuefuzhuyu capsule is improved, so as to further ensure the inherent quality and curative effect of products; 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 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 5th preparation that records, standard WS
3-B-0928-91 record prescription and quality standard:
Semen Persicae (stir-fry) 200g, Radix Angelicae Sinensis 150g, Fructus Aurantii (parched with bran) 100g, Rhizoma Chuanxiong 75g, Radix Bupleuri 50g, Flos Carthami 150g, Radix Achyranthis Bidentatae 150g, Radix Paeoniae Rubra 100g, Radix Rehmanniae 150g, Radix Platycodonis 75g, Radix Glycyrrhizae 50g
Method for making: above ten simply, and Semen Persicae 100g, Radix Angelicae Sinensis, Radix Paeoniae Rubra, Fructus Aurantii, Rhizoma Chuanxiong, Radix Bupleuri are ground into fine powder, sieves, mixing, the five tastes such as all the other Flos Carthamis and Semen Persicae 100g decoct with water three times, filter, merging filtrate, being condensed into relative density is the thick paste of 1.15-1.25 (65-70 ℃), with above-mentioned powder mixing, makes granule, oven dry, pulverize, sieve, promptly encapsulated.
Semen Persicae (stir-fry), Radix Angelicae Sinensis, Radix Bupleuri, Rhizoma Chuanxiong, Fructus Aurantii (parched with bran) microscopical identification, thin layer chromatography that prescription is set in the standard differentiate in the prescription whether contain Fructus Aurantii (hesperidin)
XUEFU ZHUYU JIAONANG was recorded after the revision standard " the Sanitation Ministry medicine standard " the 16 51 pages in 1998, standard numbering: WS
3-B-3049-98 puts down in writing quality standard:
Semen Persicae (stir-fry), Radix Angelicae Sinensis, Radix Bupleuri, Rhizoma Chuanxiong, Fructus Aurantii (parched with bran) microscopical identification, thin layer chromatography that prescription is set in the standard differentiate in the prescription whether contain Fructus Aurantii (hesperidin), Radix Paeoniae Rubra composition; High performance liquid chromatography (appendix VI D) is measured the content of paeoniflorin in the prescription, and every of this product contains paeoniflorin (C
23H
28O
11) must not be lower than 0.24mg
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 paeoniflorin 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.
Summary of the invention
The objective of the invention is to the present invention is directed to the deficiencies in the prior art, adopt new means that the quality of XUEFU ZHUYU JIAONANG is controlled, particularly set up in the preparation detection method that three kinds of compositions carry out assay simultaneously, measured the content of amygdaloside in this medicine, peoniflorin, naringin with high-efficient liquid phase technique simultaneously; Increase the thin layer chromatography qualitative identification method of Radix Bupleuri, Radix Glycyrrhizae two flavor medical materials, make sample treatment quicker, easy, guaranteed this compound preparation higher quality standard level.Provide a kind of new method of quality control of XUEFU ZHUYU JIAONANG, with the accuracy and the advance of the examination criteria of ensuring the quality of products.
In order to reach the technical scheme that purpose of the present invention adopts be: a kind of method of quality control of XUEFU ZHUYU JIAONANG, wherein said pharmaceutical formulation are by Chinese crude drug:
Semen Persicae (stir-fry) 200g, Radix Angelicae Sinensis 150g, Fructus Aurantii (parched with bran) 100g, Rhizoma Chuanxiong 75g, Radix Bupleuri 50g, Flos Carthami 150g, Radix Achyranthis Bidentatae 150g, Radix Paeoniae Rubra 100g, Radix Rehmanniae 150g, Radix Platycodonis 75g, Radix Glycyrrhizae 50g form, and above-mentioned raw materials is made 1000 capsules altogether,
Method for making: get Chinese crude drug Semen Persicae 100g, Radix Angelicae Sinensis 150g, Radix Paeoniae Rubra 100g, Fructus Aurantii (parched with bran) 100g, Rhizoma Chuanxiong 75g, Radix Bupleuri 50g, the above-mentioned raw materials Six-element is ground into fine powder, sieve, mixing, the five tastes such as all the other Flos Carthami 150g, Radix Achyranthis Bidentatae 150g, Radix Rehmanniae 150g, Radix Platycodonis 75g, Radix Glycyrrhizae 50g and Semen Persicae 100g decoct with water three times, filter, merging filtrate, being condensed into relative density is the thick paste of 1.15～1.25 (65～70 ℃), with above-mentioned powder mixing, make granule, oven dry is pulverized, sieve, make 1000 capsules, that is, it is characterized in that: the step of its method is:
(1) be control medicinal material with Radix Bupleuri, Radix Glycyrrhizae, thin layer chromatography differentiates in the XUEFU ZHUYU JIAONANG prescription whether contain Radix Bupleuri, licorice ingredient;
(2) with amygdaloside (C
20H
27NO
11), peoniflorin (C
23H
28O
11), naringin (C
27H
32O
14) be reference substance, high performance liquid chromatography detect amygdaloside in the XUEFU ZHUYU JIAONANG prescription,, the content of peoniflorin, naringin.
The method of quality control of described XUEFU ZHUYU JIAONANG is characterized in that:
Described thin layer chromatography differentiates that the method that whether contains the Radix Bupleuri composition in the XUEFU ZHUYU JIAONANG prescription is: the preparation of need testing solution: the content of getting this product 10-40 grain, porphyrize, get 2.0-10.0g, add methanol 20-90ml, supersound process 20-40min is put coldly, filters, the filtrate evaporate to dryness, residue adds water 10-40ml makes dissolving, extracts 3-5 time with the water-saturated n-butanol jolting, each 10-30ml, merge n-butyl alcohol liquid, with ammonia solution 30-60ml washing 1-2 time, the water 30-60ml that the reuse n-butyl alcohol is saturated washs the n-butyl alcohol evaporate to dryness 1-2 time, residue adds methanol 2-10ml makes dissolving, promptly;
The preparation of control medicinal material solution: take by weighing Radix Bupleuri control medicinal material 0.2-5g, with the need testing solution preparation method; Test according to thin layer chromatography: draw each 5-20 μ l of two kinds of solution of above-mentioned control medicinal material and test sample, put respectively on any lamellae in same silica gel G or GF254, chloroform-methanol-water is developing solvent, with chloroform: lower floor's solution of methanol: water=11-15: 5-9: 1-3, launch, take out, dry, spray is with 40% sulfuric acid solution of 2-4% paradime thylaminobenzaldehyde, and it is clear to be heated to the speckle colour developing at 100-110 ℃.In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the speckle of same color;
Described thin layer chromatography differentiates that the method that whether contains licorice ingredient in the XUEFU ZHUYU JIAONANG prescription is: the preparation of need testing solution: get the content of this product 10-40 grain, porphyrize is got 2.0-10.0g, add methanol 10-100ml, supersound process 10-40min filters, the filtrate evaporate to dryness, residue adds water 10-50ml makes dissolving, extracts 2-4 time with the ether jolting, each 10-50ml, discard ether solution, the jolting of reuse water-saturated n-butanol is extracted 2-4 time, and each 10-50ml merges n-butyl alcohol liquid; With the saturated water washing of n-butyl alcohol 2-4 time, each 10-50ml; Discard water liquid, n-butyl alcohol liquid evaporate to dryness, residue add methanol 2-10ml makes dissolving promptly.
The preparation of control medicinal material solution: take by weighing Radix Glycyrrhizae control medicinal material 0.2-5g, with the need testing solution preparation method; Test according to thin layer chromatography: draw each 5-20 μ l of two kinds of solution of above-mentioned control medicinal material and test sample, put respectively on any lamellae in same silica gel G or GF254, chloroform-methanol-water is developing solvent, with chloroform: lower floor's solution of methanol: water=11-15: 4-8: 1-3, launch, take out, dry, spray is with the 5-10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 100-110 ℃; In the test sample chromatograph, be on the control medicinal material chromatograph relevant position, show the speckle of same color.
The method of quality control of described 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 octadecylsilane chemically bonded silica is filler; 0.01-1% glacial acetic acid aqueous solution-acetonitrile is a mobile phase, and the regulation in the according to the form below 1 is carried out gradient elution; Flow velocity: 0.5-1.0ml/min; Column temperature 20-45 ℃; (drift tube temperature is 90～115 ℃ to evaporative light scattering detector; Air velocity is 2～3L/min);
Table 1 gradient elution table
(2) preparation of reference substance solution: it is an amount of that precision takes by weighing amygdaloside (put in the phosphorus pentoxide vacuum drying apparatus dry more than 12 hours), peoniflorin (putting in the phosphorus pentoxide vacuum drying apparatus dry more than 12 hours), naringin (putting 105 ℃ of dryings more than 5 hours) reference substance respectively, add in methanol or 50% methanol (V/V) or the ethanol any and make dissolving, make the mixed solution that every 1ml contains amygdaloside 10-80 μ g, peoniflorin 100-180 μ g, naringin 100-180 μ g;
(3) preparation of need testing solution: get the content of this product 10-30 grain, mixing, porphyrize, get 0.2-3g, accurate claim surely, place 10,25 or the 50ml measuring bottle, accurate any 9-49ml that adds in methanol, 50% methanol or the ethanol, supersound extraction 10-60min, put coldly, add methanol or aqueous methanol or aquiferous ethanol, shake up to scale, filter with 0.45 μ m filter membrane, promptly;
(4) algoscopy: accurate respectively reference substance solution and each 5-20 μ l of need testing solution of drawing, inject chromatograph of liquid, measure the content of amygdaloside, peoniflorin, naringin simultaneously.
The invention beneficial effect: being provided with Radix Bupleuri, Radix Glycyrrhizae in the quality standard is control medicinal material, and thin layer chromatography differentiates in the XUEFU ZHUYU JIAONANG prescription whether contain Radix Bupleuri, licorice ingredient; With amygdaloside (C
20H
27NO
11), peoniflorin (C
23H
28O
11), naringin (C
27H
32O
14) be reference substance, high performance liquid chromatography detect amygdaloside in the XUEFU ZHUYU JIAONANG prescription,, the method for inspection of the content of peoniflorin, naringin, changed the situation of single index component content control compound recipe quality in the primary standard, 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 thin layer that the invention provides Radix Bupleuri and Radix Glycyrrhizae is differentiated, set up the HPLC detection method that amygdaloside, peoniflorin, three kinds of compositions of naringin are measured simultaneously, through repeated trials repeatedly, confirmation method is easy, the result is accurate, can be used as the index of XUEFU ZHUYU JIAONANG quality control and investigation technology stability.
Example 1: get Chinese crude drug Semen Persicae 100g, Radix Angelicae Sinensis 150g, Radix Paeoniae Rubra 100g, Fructus Aurantii (parched with bran) 100g, Rhizoma Chuanxiong 75g, Radix Bupleuri 50g, the above-mentioned raw materials Six-element is ground into fine powder, sieve, mixing, the five tastes such as all the other Flos Carthami 150g, Radix Achyranthis Bidentatae 150g, Radix Rehmanniae 150g, Radix Platycodonis 75g, Radix Glycyrrhizae 50g and Semen Persicae 100g decoct with water three times, filter, merging filtrate, being condensed into relative density is the thick paste of 1.15～1.25 (65～70 ℃), with above-mentioned powder mixing, make granule, oven dry is pulverized, and sieves, make 1000 capsules, promptly; The method of quality control of this medicine comprises the following steps:
(1) measures amygdaloside (C in this medicine simultaneously with high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005)
20H
27NO
11), peoniflorin (C
23H
28O
11), naringin (C
27H
32O
14) content:
A. chromatographic condition: with octadecylsilane chemically bonded silica is filler; Acetonitrile-1% glacial acetic acid solution is eluent gradient eluting (gradient condition is from 0-50min, and the acetonitrile ratio changes to 70% from 5%), and (drift tube temperature is 110 ℃ to evaporative light scattering detector; Air velocity is 2.5L/min);
B. the preparation of reference substance solution: precision takes by weighing amygdaloside (put in the phosphorus pentoxide vacuum drying apparatus dry 12 hours), peoniflorin (put in the phosphorus pentoxide vacuum drying apparatus dry 12 hours), naringin (putting 105 ℃ of dryings 5 hours) reference substance 10mg, 17mg, 17mg respectively, put respectively in the 25ml measuring bottle, add 50% methanol (V/V) and make dissolving and be diluted to scale, shake up; Precision is measured 3ml, 5ml respectively, 5ml puts in the 25ml measuring bottle, adds 50% methanol to scale, shakes up, promptly.
C. the preparation of need testing solution: get 10 of this product, get content, mixing, porphyrize is got 0.5g, the accurate title, decide, and places the 25ml measuring bottle, the accurate 50% methanol 24ml that adds, and supersound extraction 30min is put cold, add 50% methanol to scale, shake up, filter with 0.45 μ m filter membrane, promptly;
D. the content assaying method of amygdaloside, peoniflorin, naringin: accurate respectively each the 20 μ l of reference substance solution and need testing solution that draw, the injection chromatograph of liquid is measured the content of amygdaloside, peoniflorin, naringin simultaneously;
(2) this medicine Chinese crude drug Radix Bupleuri is differentiated with thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B):
A. the preparation of need testing solution: get 20 of this product, get the content porphyrize, get 4.0g, add methanol 30ml, supersound process 30min is put cold, filter, filtrate evaporate to dryness, residue add water 30ml makes dissolving, extract 3 times with the water-saturated n-butanol jolting, each 20ml merges 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, promptly.
B. the preparation of control medicinal material solution: take by weighing Radix Bupleuri control medicinal material 0.5g, with the need testing solution preparation method.
C. test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005): draw each 5-20 μ l of two kinds of solution of above-mentioned control medicinal material and test sample, put respectively on same silica gel g thin-layer plate, being developing solvent in chloroform-methanol-water (13: 7: 2) lower floor, launch, take out, dry, spray is with 40% sulfuric acid solution of 2% paradime thylaminobenzaldehyde, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, be on the control medicinal material chromatograph relevant position, show the speckle of same color.
(3) this medicine Chinese crude drug Radix Glycyrrhizae is differentiated with thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B):
A. the preparation of need testing solution: get 20 of this product, get the content porphyrize, get 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 makes dissolving promptly.
B. the preparation of control medicinal material solution: take by weighing Radix Glycyrrhizae control medicinal material 0.2-5g, with the need testing solution preparation method.
C. test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005): draw each 5-20 μ l of two kinds of solution of above-mentioned control medicinal material and test sample, put respectively on any lamellae in same silica gel G or GF254, with chloroform-methanol-water (13: 6: 2) lower floor solution is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to speckle colour developing at 105 ℃.In the test sample chromatograph, be on the control medicinal material chromatograph relevant position, show the speckle of same color.
Example 2: get Chinese crude drug Semen Persicae 100g, Radix Angelicae Sinensis 150g, Radix Paeoniae Rubra 100g, Fructus Aurantii (parched with bran) 100g, Rhizoma Chuanxiong 75g, Radix Bupleuri 50g, the above-mentioned raw materials Six-element is ground into fine powder, sieve, mixing, the five tastes such as all the other Flos Carthami 150g, Radix Achyranthis Bidentatae 150g, Radix Rehmanniae 150g, Radix Platycodonis 75g, Radix Glycyrrhizae 50g and Semen Persicae 100g decoct with water three times, filter, merging filtrate, being condensed into relative density is the thick paste of 1.15～1.25 (65～70 ℃), with above-mentioned powder mixing, make granule, oven dry is pulverized, and sieves, make 1000 capsules, promptly; The method of quality control of this medicine comprises the following steps:
(1) measures amygdaloside (C in this medicine simultaneously with high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005)
20H
27NO
11), peoniflorin (C
23H
28O
11), naringin (C
27H
32O
14) content:
A. chromatographic condition: with octadecylsilane chemically bonded silica is filler; Acetonitrile-0.8% glacial acetic acid solution is eluent gradient eluting (gradient condition is at 0-50min, and the acetonitrile ratio changes to 45% from 5%), and (drift tube temperature is 105 ℃ to evaporative light scattering detector; Air velocity is 2.0L/min);
B. the preparation of reference substance solution: precision takes by weighing amygdaloside (put in the phosphorus pentoxide vacuum drying apparatus dry 12 hours), peoniflorin (put in the phosphorus pentoxide vacuum drying apparatus dry 12 hours), naringin (putting 105 ℃ of dryings 5 hours) reference substance 8mg, 12mg, 12mg respectively, put respectively in the 25ml measuring bottle, add 50% methanol (V/V) and make dissolving and be diluted to scale, shake up; Precision is measured 3ml, 5ml respectively, 5ml puts in the 25ml measuring bottle, adds 50% methanol to scale, shakes up, promptly.
C. the preparation of need testing solution: get 10 of this product, get content, mixing, porphyrize is got 1.0g, the accurate title, decide, and places the 25ml measuring bottle, the accurate 50% methanol 24ml that adds, and supersound extraction 20min is put cold, add 50% methanol to scale, shake up, filter with 0.45 μ m filter membrane, promptly;
D. the content assaying method of amygdaloside, peoniflorin, naringin: accurate respectively each the 10 μ l of reference substance solution and need testing solution that draw, the injection chromatograph of liquid is measured the content of amygdaloside, peoniflorin, naringin simultaneously;
(2) this medicine Chinese crude drug Radix Bupleuri is differentiated with thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B):
A. the preparation of need testing solution: get 20 of this product, get the content porphyrize, get 5.0g, add methanol 40ml, supersound process 20min is put cold, filter, filtrate evaporate to dryness, residue add water 40ml makes dissolving, extract 2 times with the water-saturated n-butanol jolting, each 30ml merges 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 2 times, residue adds methanol 5ml makes dissolving, promptly.
B. the preparation of control medicinal material solution: take by weighing Radix Bupleuri control medicinal material 0.5g, with the need testing solution preparation method.
C. test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005): draw each 10 μ l of two kinds of solution of above-mentioned control medicinal material and test sample, put respectively on same silica gel g thin-layer plate, being developing solvent in chloroform-methanol-water (14: 7: 1) lower floor, launch, take out, dry, spray is with 40% sulfuric acid solution of 2% paradime thylaminobenzaldehyde, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, be on the control medicinal material chromatograph relevant position, show the speckle of same color.
(3) this medicine Chinese crude drug Radix Glycyrrhizae is differentiated with thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B):
A. the preparation of need testing solution: get 20 of this product, get the content porphyrize, get 6.0g, add methanol 50ml, supersound process 40min filters, the filtrate evaporate to dryness, residue adds water 30ml 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 3 times, each 20ml; Discard water liquid, n-butyl alcohol liquid evaporate to dryness, residue add methanol makes dissolving promptly.
B. the preparation of control medicinal material solution: take by weighing Radix Glycyrrhizae control medicinal material 3g, with the need testing solution preparation method.
C. test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005): draw each 10 μ l of two kinds of solution of above-mentioned control medicinal material and test sample, put respectively on any lamellae in same silica gel G or GF254, with chloroform-methanol-water (14: 7: 2) lower floor solution is developing solvent, launch, take out, dry, spray is with 5% ethanol solution of sulfuric acid, and it is clear to be heated to speckle colour developing at 105 ℃.In the test sample chromatograph, be on the control medicinal material chromatograph relevant position, show the speckle of same color.
Claims (3)
1. the method for quality control of an XUEFU ZHUYU JIAONANG, wherein said pharmaceutical formulation is by Chinese crude drug: Semen Persicae (parched) 200g, Radix Angelicae Sinensis 150g, stir-baked Fructus Aurantii in bran 100g, Rhizoma Chuanxiong 75g, Radix Bupleuri 50g, Flos Carthami 150g, Radix Achyranthis Bidentatae 150g, Radix Paeoniae Rubra 100g, Radix Rehmanniae 150g, Radix Platycodonis 75g, Radix Glycyrrhizae 50g forms, above-mentioned raw materials is made 1000 capsules altogether, method for making: get Chinese crude drug Semen Persicae 100g, Radix Angelicae Sinensis 150g, Radix Paeoniae Rubra 100g, stir-baked Fructus Aurantii in bran 100g, Rhizoma Chuanxiong 75g, Radix Bupleuri 50g, the above-mentioned raw materials Six-element is ground into fine powder, sieve, mixing, all the other Flos Carthami 150g, Radix Achyranthis Bidentatae 150g, Radix Rehmanniae 150g, Radix Platycodonis 75g, the five tastes such as Radix Glycyrrhizae 50g and Semen Persicae 100g decoct with water three times, filter, merging filtrate, be condensed into 65～70 ℃ of relative densities and be 1.15～1.25 thick paste,, make granule with above-mentioned powder mixing, oven dry, pulverize, sieve, make 1000 capsules, that is, it is characterized in that: the step of its method is:
(1) be control medicinal material with Radix Bupleuri, Radix Glycyrrhizae, thin layer chromatography differentiates in the XUEFU ZHUYU JIAONANG prescription whether contain Radix Bupleuri, licorice ingredient;
(2) with amygdaloside (C
20H
27NO
11), peoniflorin (C
23H
28O
11), naringin (C
27H
32O
14) be reference substance, high performance liquid chromatography detects the content of amygdaloside, peoniflorin, naringin in the XUEFU ZHUYU JIAONANG prescription.
2. the method for quality control of XUEFU ZHUYU JIAONANG according to claim 1, it is characterized in that: described thin layer chromatography differentiates that the method that whether contains the Radix Bupleuri composition in the XUEFU ZHUYU JIAONANG prescription is: the preparation of need testing solution: the content of getting this product 10-40 grain, porphyrize, get 2.0-10.0g, add methanol 20-90ml, supersound process 20-40min, put cold, filter, filtrate evaporate to dryness, residue add water 10-40ml makes dissolving, extract 3-5 time with the water-saturated n-butanol jolting, each 10-30ml merges n-butyl alcohol liquid, with ammonia solution 30-60ml washing 1-2 time, the water 30-60ml that the reuse n-butyl alcohol is saturated washs 1-2 time, n-butyl alcohol evaporate to dryness, residue add methanol 2-10ml makes dissolving, promptly; The preparation of control medicinal material solution: take by weighing Radix Bupleuri control medicinal material 0.2-5g, with the need testing solution preparation method; Test according to thin layer chromatography: draw each 5-20 μ l of two kinds of solution of above-mentioned control medicinal material and test sample, put respectively on any lamellae in same silica gel G or GF254, chloroform-methanol-water is developing solvent, with chloroform: lower floor's solution of methanol: water=11-15: 5-9: 1-3, launch, take out, dry, spray is with 40% sulfuric acid solution of 2-4% paradime thylaminobenzaldehyde, and it is clear to be heated to the speckle colour developing at 100-110 ℃; In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the speckle of same color;
Described thin layer chromatography differentiates that the method that whether contains licorice ingredient in the XUEFU ZHUYU JIAONANG prescription is: the preparation of need testing solution: get the content of this product 10-40 grain, porphyrize is got 2.0-10.0g, add methanol 10-100ml, supersound process 10-40min filters, the filtrate evaporate to dryness, residue adds water 10-50ml makes dissolving, extracts 2-4 time with the ether jolting, each 10-50ml, discard ether solution, the jolting of reuse water-saturated n-butanol is extracted 2-4 time, and each 10-50ml merges n-butyl alcohol liquid; With the saturated water washing of n-butyl alcohol 2-4 time, each 10-50ml; Discard water liquid, n-butyl alcohol liquid evaporate to dryness, residue add methanol 2-10ml makes dissolving promptly;
The preparation of control medicinal material solution: take by weighing Radix Glycyrrhizae control medicinal material 0.2-5g, with the need testing solution preparation method; Test according to thin layer chromatography: draw each 5-20 μ l of two kinds of solution of above-mentioned control medicinal material and test sample, put respectively on any lamellae in same silica gel G or GF254, chloroform-methanol-water is developing solvent, with chloroform: lower floor's solution of methanol: water=11-15: 4-8: 1-3, launch, take out, dry, spray is with the 5-10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 100-110 ℃; In the test sample chromatograph, be on the control medicinal material chromatograph relevant position, show the speckle of same color.
3. the method for quality control of 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 octadecylsilane chemically bonded silica is filler; 0.01-1% glacial acetic acid aqueous solution-acetonitrile is a mobile phase, and the regulation in the according to the form below 1 is carried out gradient elution; Flow velocity: 0.5-1.0ml/min; Column temperature 20-45 ℃; The evaporative light scattering detector drift tube temperature is 90～115 ℃; Air velocity is 2～3L/min;
Table 1 gradient elution table
(2) preparation of reference substance solution: respectively precision take by weighing amygdaloside put in the phosphorus pentoxide vacuum drying apparatus dry more than 12 hours, peoniflorin put dry more than 12 hours in the phosphorus pentoxide vacuum drying apparatus, naringin put 105 ℃ of dryings more than 5 hours reference substance an amount of, add in methanol or 50% methanol (V/V) or the ethanol any and make dissolving, make the mixed solution that every 1ml contains amygdaloside 10-80 μ g, peoniflorin 100-180 μ g, naringin 100-180 μ g;
(3) preparation of need testing solution: get the content of this product 10-30 grain, mixing, porphyrize, get 0.2-3g, accurate claim surely, place 10,25 or the 50ml measuring bottle, accurate any 9-49ml that adds in methanol, 50% methanol or the ethanol, supersound extraction 10-60min, put coldly, add methanol or aqueous methanol or aquiferous ethanol, shake up to scale, filter with 0.45 μ m filter membrane, promptly;
(4) algoscopy: accurate respectively reference substance solution and each 5-20 μ l of need testing solution of drawing, inject chromatograph of liquid, measure the content of amygdaloside, peoniflorin, naringin simultaneously.
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