CN103983734B - A kind of detection method preparing Chanhou Zhuyu Capsule - Google Patents
A kind of detection method preparing Chanhou Zhuyu Capsule Download PDFInfo
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Abstract
The present invention relates to a kind of detection method preparing Chanhou Zhuyu Capsule, the method relates to the indentification by TLC of Ligusticum wallichii, Radix Angelicae Sinensis, motherwort, the high performance liquid chromatography assay of forulic acid and limit thereof.
Description
Technical field
The present invention relates to a kind of detection method preparing Chanhou Zhuyu Capsule.
Background technology
The remaining blood that postpartum after parturient childbirth, extravasated blood was mainly left in uterus and turbid liquid, be not normal by QI-blood circulation, stagnation of QI and blood causes, and is one of gynemetrics's common clinical.
The traditional Chinese medical science is thought, this pathology mainly QI-blood circulation is not normal, stagnation of QI and blood.Doctor trained in Western medicine is thought, its cause of disease mainly uterine involution is incomplete, and when part placenta, fetal membrane is residual or infect and affect uterine contractile and recovery; Or puerpera as suffered from chronic disease, excessive blood loss, excessively tired, physique fails to recover, or the local factor such as uterus overexpansion, fibroid, all can affect uterine involution incomplete.Secondly, cesarean postoperate, when uterine wall disruption of wound, operation, hemostasis is thoroughly or because of postoperative infection, affect uterine involution and causes bleeding incessantly.
Therefore, at present to women's extravasated blood in postpartum, doctor trained in Western medicine generally adopts accelerates uterine contraction with hemostasis, and enriches blood, continue with microbiotic infection control etc., though through treatment energy relief of symptoms, have certain bad reaction, result for the treatment of is not satisfactory, although the effect of getting instant result can be reached when treating this disease, but western medicine women uterus in postpartum extravasated blood, toxic and side effect are larger, easy recurrent exerbation, and fundamentally can not thoroughly cure this disease.China's traditional medicine utilizes treatment by Chinese herbs women uterus in postpartum extravasated blood, not only can reach the effect of hemostasis rapidly, the more important thing is and can also carry out double recuperation to human body, thus reach equilibrium between yin and yang, qi and blood is normally run, reach the object of hemostasis.
At present, domestic had in related application such as 2013107103201 namely disclose a kind of puerperal blood clot dispersing particle and preparation method thereof, but preparation method disclosed in this patent incomplete, also lack the effective detection method ensureing product quality.And well-known, the mutually auxiliary restriction or checking relation in five elements of Chinese medicinal ingredients, very high to the requirement of preparation technology, otherwise be difficult to the result for the treatment of reaching expection.Therefore, in currently available technology, the preparation method of Related product cannot meet the needs of actual production.
Summary of the invention
The present invention is just from prior art, and provide a kind of detection method preparing Chanhou Zhuyu Capsule, it is suitable in widespread use actual production process.
The detection method preparing Chanhou Zhuyu Capsule provided by the invention, wherein said Chanhou Zhuyu Capsule is made up of motherwort, Radix Angelicae Sinensis, Ligusticum wallichii, baked ginger, and described Chanhou Zhuyu Capsule adopts following preparation method to obtain:
Motherwort 1248g Radix Angelicae Sinensis 156g Ligusticum wallichii 178g baked ginger 78g
Above four tastes, get motherwort, Radix Angelicae Sinensis, each 20g of Ligusticum wallichii are ground into fine powder, for subsequent use, residue Radix Angelicae Sinensis, Ligusticum wallichii and baked ginger add 10 times of water gaging distillation extractions 3 hours, collect volatile oil, the dregs of a decoction add 10 times amount, 8 times amount soak by water secondaries respectively with residue motherwort, 2 hours first times, second time 1 hour, filter, filtrate merges, and is concentrated into relative density is determined as 1.35 thick paste at 50 DEG C, add above-mentioned fine powder, mixing, dries, particle processed, dry again, add the volatile oil such as Radix Angelicae Sinensis, mixing, encapsulated, make this product 1000, to obtain final product;
The detection method preparing described Chanhou Zhuyu Capsule is:
(1) this product 10 is got, incline and content, porphyrize, add the ultrasonic process of absolute ethyl alcohol 10ml 20 minutes, filter, filtrate is as need testing solution, separately get Radix Angelicae Sinensis, the each 0.5g of Ligusticum wallichii control medicinal material, add absolute ethyl alcohol 10ml respectively, be made in the same way of control medicinal material solution, test according to thin-layered chromatography, draw above-mentioned need testing solution 10 μ l, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, with n-hexane-ethyl acetate (9: 1) for developping agent, launch, take out, dry, inspect under ultraviolet light, in test sample chromatogram, on the position corresponding to control medicinal material chromatogram, the fluorescence spot of aobvious same color,
(2) this product 5 is got, incline and content, porphyrize, add absolute ethyl alcohol 30ml refluxing extraction 1 hour, filter, filtrate adds activated charcoal 0.5g, ultrasonic process 10 minutes, filter, filtrate evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution, separately get motherwort control medicinal material 1g, add absolute ethyl alcohol 30ml refluxing extraction 1 hour, filter, filtrate adds activated charcoal 0.5g, ultrasonic process 10 minutes, filter, filtrate evaporate to dryness, residue adds methyl alcohol 0.5ml makes dissolving, medicinal material solution in contrast, get stachydrine hydrochloride reference substance again to add methyl alcohol and make every 1ml containing the reference substance solution of 1mg, test according to thin-layered chromatography, draw each 10 μ l of above-mentioned solution respectively, put respectively on same silica gel g thin-layer plate, with acetone-absolute ethyl alcohol-hydrochloric acid (10: 6: 1) for developping agent, launch, take out, dry, put 105 DEG C of heating 5 minutes, spray is with rare bismuth potassium iodide test solution, inspect in the sunlight, in test sample chromatogram, on corresponding to reference substance chromatogram and that control medicinal material chromatogram is corresponding position, the spot of aobvious same color,
(3) assay
Chromatographic condition and system suitability octadecylsilane chemically bonded silica are filling agent; Acetonitrile-1% glacial acetic acid solution (19: 81) is mobile phase; Determined wavelength is 323nm; Column temperature 40 DEG C; Flow velocity 0.8ml/min, number of theoretical plate calculates should be not less than 3000 by forulic acid peak,
The preparation of reference substance solution gets forulic acid reference substance in right amount, accurately weighed, adds 50% methyl alcohol and makes the solution of every 1ml containing 10 μ g, to obtain final product,
This product 30 is got in the preparation of need testing solution, and porphyrize, inclines and content, accurately weighed, porphyrize, gets about 4g, accurately weighed, and precision adds methyl alcohol 50ml, weighed weight, ultrasonic process 50 minutes, lets cool, more weighed weight, supply the weight of less loss with methyl alcohol, shake up, filter, accurate absorption subsequent filtrate 15ml, puts in 25ml measuring bottle, is diluted with water to scale, shake up, to obtain final product
Determination method is accurate respectively draws contrast solution and each 20 μ l of need testing solution, injection liquid chromatography, measures, to obtain final product.
Preferably, every described Chanhou Zhuyu Capsule containing Radix Angelicae Sinensis and Ligusticum wallichii with forulic acid (C
10h
10o
4) meter, be no less than 30 μ g.
Preferably, the power of ultrasonic process in assay process is 120W, and frequency is 59KHz.
The present invention is found by a large amount of creative work, and Radix Angelicae Sinensis in prescription, Ligusticum wallichii have to enrich blood invigorates blood circulation, and the effect before menstruation regulating is only all main containing forulic acid.Therefore, the present invention adopts high performance liquid chromatography to carry out quantitatively forulic acid in preparation, and method is easy, sensitive, can be used as the key element controlling and investigate this quality.
On the other hand, preparing in Chanhou Zhuyu Capsule actual production preparation process, adopting detection method of the present invention easy, sensitive, the quality of precisely control product can also realized while effective production control cost, be suitable in widespread use actual production process.
Accompanying drawing explanation
The chromatogram of the TLC collection of illustrative plates of Fig. 1 Radix Angelicae Sinensis, Ligusticum wallichii
The TLC collection of illustrative plates of Fig. 2 motherwort
Embodiment
Below, the specific embodiment of the detection method of Chanhou Zhuyu Capsule of the present invention is provided.
Embodiment 1,
Motherwort 1248g Radix Angelicae Sinensis 156g Ligusticum wallichii 178g baked ginger 78g
Preparation method:
Above four tastes, get motherwort, Radix Angelicae Sinensis, each 20g of Ligusticum wallichii are ground into fine powder, for subsequent use, residue Radix Angelicae Sinensis, Ligusticum wallichii and baked ginger add 10 times of water gaging distillation extractions 3 hours, collect volatile oil, the dregs of a decoction add 10 times amount, 8 times amount soak by water secondaries respectively with residue motherwort, 2 hours first times, second time 1 hour, filter, filtrate merges, and is concentrated into the thick paste of relative density 1.35 (50 DEG C), add above-mentioned fine powder, mixing, dries, particle processed, dry again, add the volatile oil such as Radix Angelicae Sinensis, mixing, encapsulated, make 1000, to obtain final product.
Detection method:
(1) get this product 10, incline and content, porphyrize, add the ultrasonic process of absolute ethyl alcohol 10ml 20 minutes, filter, filtrate is as need testing solution.Separately get Radix Angelicae Sinensis, each 0.5g of Ligusticum wallichii control medicinal material, add absolute ethyl alcohol 10ml respectively, be made in the same way of control medicinal material solution.According to thin-layered chromatography (Chinese Pharmacopoeia version in 2010 annex VIB) test, draw above-mentioned need testing solution 10 μ l, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, with n-hexane-ethyl acetate (9: 1) for developping agent, launch, take out, dry.Inspect under ultraviolet light (365nm).In test sample chromatogram, on the position corresponding to control medicinal material chromatogram, the fluorescence spot of aobvious same color.
(2) get this product 5, incline and content, porphyrize, add absolute ethyl alcohol 30ml refluxing extraction 1 hour, filter, filtrate adds activated charcoal 0.5g, ultrasonic process 10 minutes, and filter, filtrate evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution.Separately get motherwort control medicinal material 1g, add absolute ethyl alcohol 30ml refluxing extraction 1 hour, filter, filtrate adds activated charcoal 0.5g, ultrasonic process 10 minutes, and filter, filtrate evaporate to dryness, residue adds methyl alcohol 0.5ml makes dissolving, medicinal material solution in contrast.Get stachydrine hydrochloride reference substance again to add methyl alcohol and make every 1ml containing the reference substance solution of 1mg.Test according to thin-layered chromatography (Chinese Pharmacopoeia version in 2010 annex VIB), draw each 10 μ l of above-mentioned solution respectively, put respectively on same silica gel g thin-layer plate, with acetone-absolute ethyl alcohol-hydrochloric acid (10: 6: 1) for developping agent, launch, take out, dry, put 105 DEG C of heating 5 minutes, spray with rare bismuth potassium iodide test solution, inspect in the sunlight.In test sample chromatogram, on corresponding to reference substance chromatogram and that control medicinal material chromatogram is corresponding position, the spot of aobvious same color.
(3) assay
Chromatographic condition and system suitability octadecylsilane chemically bonded silica are filling agent; Acetonitrile-1% glacial acetic acid solution (19: 81) is mobile phase; Determined wavelength is 323nm.Number of theoretical plate calculates should be not less than 3000 by forulic acid peak.
The preparation of reference substance solution gets forulic acid reference substance in right amount, accurately weighed, adds 50% methyl alcohol and makes the solution of every 1ml containing 10 μ g, to obtain final product.
This product 30 is got in the preparation of need testing solution, and porphyrize, inclines and content, accurately weighed, porphyrize, gets about 4g, accurately weighed, and precision adds methyl alcohol 50ml, weighed weight, ultrasonic process (power 120W, frequency 59KHz) 50 minutes, lets cool, weighed weight again, supplies the weight of less loss, shakes up with methyl alcohol, filter, accurate absorption subsequent filtrate 15ml, puts in 25ml measuring bottle, be diluted with water to scale, shake up, to obtain final product.
Determination method is accurate respectively draws contrast solution and each 20 μ l of need testing solution, injection liquid chromatography, measures, to obtain final product.
This product every in forulic acid (C10H1004), must not be less than 30 μ g containing Radix Angelicae Sinensis and Ligusticum wallichii.
Experimental example 1: the indentification by TLC of Radix Angelicae Sinensis, Ligusticum chuanxiong Hort
With Radix Angelicae Sinensis, Ligusticum wallichii control medicinal material, for positive control, (Nat'l Pharmaceutical & Biological Products Control Institute provides, lot number 120927-200310,120918-200406), with normal hexane-ethyl acetate (9: 1) for expanding into, spot 365nm after expansion inspects, fluorescent spot point rounding, good separating effect.Separately get in prescription and do not make negative sample containing other medicinal material of Radix Angelicae Sinensis, Ligusticum wallichii by preparation method, then make negative sample solution by need testing solution preparation method.Through three batch samples and negative control experiments, negative noiseless.
Wherein in accompanying drawing 1,1, Radix Angelicae Sinensis control medicinal material 2, Ligusticum wallichii control medicinal material 3,4,5 three batch sample 6, negative sample.
Experimental example 2: the indentification by TLC of motherwort medicinal material
With stachydrine hydrochloride reference substance (Nat'l Pharmaceutical & Biological Products Control Institute, lot number 110712-200306) and motherwort control medicinal material (Nat'l Pharmaceutical & Biological Products Control Institute, lot number 1120912-200306) be positive control, once I was compared: n-butyl alcohol-hydrochloric acid-water (4: 1: 0.5), II: the developping agents such as acetone-absolute ethyl alcohol-hydrochloric acid (10: 6: 1), spot rounding after wherein launching with developping agent II, good separating effect.Other medicinal material separately got not containing motherwort in prescription is made negative sample by preparation method, then is made negative sample solution by need testing solution preparation method.Through three batch samples and negative control experiments, negative noiseless.
Wherein in accompanying drawing 2,1, stachydrine hydrochloride reference substance 2, motherwort control medicinal material 3,4,5 three batch sample 6, negative sample.
Experimental example 3: ferulaic acid content measures
This product is made up of benefit female stroke, Radix Angelicae Sinensis, Ligusticum wallichii, baked ginger four traditional Chinese medicine.Radix Angelicae Sinensis in prescription, Ligusticum wallichii have to enrich blood invigorates blood circulation, the effect before menstruation regulating only, all main containing forulic acid.Now adopt high performance liquid chromatography to carry out quantitatively forulic acid in preparation, method is easy, sensitive, can be used as the method controlling and investigate this product inherent quality.
(1) instrument and reagent
LC-10ADvp high performance liquid chromatograph (Shimadzu), SPD-10Avp detecting device, forulic acid reference substance (lot number 0773-9910, is provided by Nat'l Pharmaceutical & Biological Products Control Institute), acetonitrile is chromatographically pure, and it is pure that other reagent are analysis.
(2) chromatographic condition
Chromatographic column: octadecyl silane post (ODS) 4.6 × 250nm; Mobile phase: acetonitrile-1% glacial acetic acid solution (19: 81); Determined wavelength: 323nm; Column temperature 40 DEG C; Flow velocity 0.8ml/min.Forulic acid and other component all can reach and well be separated with this understanding, and the degree of separation of main peak and nearest impurity peaks is greater than 1.5.Number of theoretical plate is all greater than 3000.
(3) determination of determined wavelength
Get forulic acid reference substance solution to carry out retouching outside ultraviolet, obtain absorption curve, result maximum absorption band is 323nm, consistent with bibliographical information, therefore selects 323nm wavelength as determined wavelength.
(4) selection of mobile phase
According to data-gathering, once tested with the multiple flow visualizing of acetonitrile-1% glacial acetic acid solution different proportion, other component in result preparation can not effectively be separated with forulic acid, and acetonitrile-1% glacial acetic acid solution (19: 81) flow visualizing, forulic acid and other Component seperation complete, and it is fast to go out peak, result is satisfied
(5) preparation of need testing solution: get this product 30, porphyrize, inclines and content, accurately weighed, porphyrize, gets about 4g, accurately weighed, and precision adds methyl alcohol 50ml, weighed weight, ultrasonic process (power 120W, frequency 59KHz) 50 minutes, lets cool, weighed weight again, supplies the weight of less loss, shakes up with methyl alcohol, filter, accurate absorption subsequent filtrate 15ml, puts in 25ml measuring bottle, be diluted with water to scale, shake up, to obtain final product.
Another in experimentation, compare different ultrasonic extraction time to the impact of content results, result is as table 1.
The selection of table 1 ultrasonic extraction time
Therefore adopt ultrasonic extraction 50 minutes, can fully extract.
(6) blank test
Due to prescription motherwort, Radix Angelicae Sinensis, Ligusticum wallichii, baked ginger four traditional Chinese medicine composition, therefore get respectively by prescription and 1. lack Radix Angelicae Sinensis, Ligusticum chuanxiong Hort and 2. lack Ligusticum chuanxiong Hort and 3. lack other medicinal material of Radix Angelicae Sinensis medicinal material, make three corresponding negative samples respectively according to preparation technology, then make corresponding three negative sample solution by need testing solution under text assay item.Analyze according to chromatographic condition under text content assaying method item, result show 1. to lack Radix Angelicae Sinensis, Ligusticum chuanxiong Hort feminine gender noiseless to this law, and 2. lack the feminine gender of Ligusticum chuanxiong Hort and 3. lack the feminine gender of Radix Angelicae Sinensis medicinal material and have dry sorrow, this is because all containing forulic acid in Radix Angelicae Sinensis, Ligusticum wallichii.
(7) investigation of linear relationship
Precision takes forulic acid reference substance 11.0mg, put in 25ml measuring bottle, add methyl alcohol and make dissolving, and be diluted to scale, shake up (440 μ g/ml), accurate absorption is appropriate respectively again, is diluted to the reference substance solution of variable concentrations: 4.4 μ g/ml, 8.8 μ g/ml, 17.6 μ g/ml, 35.2 μ g/ml, 44.0 μ g/ml with 50% methanol solution.The accurate each 20ul of reference substance solution drawing above-mentioned variable concentrations, by chromatographic condition analysis in text, the results are shown in Table 2 respectively
Table 2 linear relationship investigates result
With integrating peak areas value for ordinate, forulic acid amount is horizontal ordinate drawing standard curve, calculates regression equation: Y=17759008X-220351, r=0.9996.Show that the amount of forulic acid has good linear relation within the scope of 0.088 μ g ~ 0.88 μ g.
(8) stability test
This product makes need testing solution according to text method, and accurate this need testing solution 20 of absorption μ l, injection liquid chromatography, sample introduction measures once at regular intervals, places in 5 hours, peak area basically identical (see table 3) in lucifuge.Show that 50% methanol solution of forulic acid is placed in 5 hours stable in lucifuge.
Table 3 stability test result
(9) precision test
The above-mentioned reference substance solution of accurate absorption (8.8 μ g/ml), repeat sample introduction 5 times (the results are shown in Table 4), the relative standard deviation of forulic acid area integral value is less than 2%, shows that this method precision is good.
Table 4 Precision test result
(10) reappearance test
Get same batch sample 5 parts respectively, by method test under assay item in text, measure the content of forulic acid, the results are shown in Table 5, the relative standard deviation of ferulaic acid content is less than 2%, shows that this method reappearance is good.
Table 5 reproducible test results
(11) recovery test
Adopt application of sample absorption method.Get the Chanhou Zhuyu Capsule (lot number: 20040501 with a collection of known content, content 0.17mg/g), precision takes powder and is about 2g, totally 5 parts, each forulic acid reference substance that quantitatively adds is appropriate, then method under assay item of pressing in text measures ferulaic acid content.Add forulic acid reference substance appropriate, measure the content of forulic acid by method under assay item in text, abandon the calculating recovery, the results are shown in Table 6, average recovery rate is 99.3%.Show that this method recovery is good.
Table 6 recovery test result 99.7
(12) sample determination
Get this product ten batches, by method test under assay item in text, measure the content of forulic acid in ten batch samples respectively.The results are shown in Table 7
Table 7 sample determination result
According to said determination result, consider the Radix Angelicae Sinensis in Different sources and source, that ferulic acid in Chuanxiong content has height to have is low, by forulic acid (C in this product
10h
10o
4) content is decided to be every (0.3g) must not lower than 0.03mg.
Claims (2)
1. prepare a detection method for Chanhou Zhuyu Capsule, wherein said Chanhou Zhuyu Capsule is made up of motherwort, Radix Angelicae Sinensis, Ligusticum wallichii, baked ginger, and described Chanhou Zhuyu Capsule adopts following preparation method to obtain:
Motherwort 1248g Radix Angelicae Sinensis 156g Ligusticum wallichii 178g baked ginger 78g
Above four tastes, get motherwort, Radix Angelicae Sinensis, each 20g of Ligusticum wallichii are ground into fine powder, for subsequent use, residue Radix Angelicae Sinensis, Ligusticum wallichii and baked ginger add 10 times of water gaging distillation extractions 3 hours, collect volatile oil, the dregs of a decoction add 10 times amount, 8 times amount soak by water secondaries respectively with residue motherwort, 2 hours first times, second time 1 hour, filter, filtrate merges, and is concentrated into relative density is determined as 1.35 thick paste at 50 DEG C, add above-mentioned fine powder, mixing, dries, particle processed, dry again, add the volatile oil such as Radix Angelicae Sinensis, mixing, encapsulated, make this product 1000, to obtain final product;
The detection method preparing described Chanhou Zhuyu Capsule is:
(1) this product 10 is got, incline and content, porphyrize, add the ultrasonic process of absolute ethyl alcohol 10ml 20 minutes, filter, filtrate is as need testing solution, separately get Radix Angelicae Sinensis, the each 0.5g of Ligusticum wallichii control medicinal material, add absolute ethyl alcohol 10ml respectively, be made in the same way of control medicinal material solution, test according to thin-layered chromatography, draw above-mentioned need testing solution 10 μ l, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, n-hexane-ethyl acetate with 9: 1 is developping agent, launch, take out, dry, inspect under ultraviolet light, in test sample chromatogram, on the position corresponding to control medicinal material chromatogram, the fluorescence spot of aobvious same color,
(2) this product 5 is got, incline and content, porphyrize, add absolute ethyl alcohol 30ml refluxing extraction 1 hour, filter, filtrate adds activated charcoal 0.5g, ultrasonic process 10 minutes, filter, filtrate evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution, separately get motherwort control medicinal material 1g, add absolute ethyl alcohol 30ml refluxing extraction 1 hour, filter, filtrate adds activated charcoal 0.5g, ultrasonic process 10 minutes, filter, filtrate evaporate to dryness, residue adds methyl alcohol 0.5ml makes dissolving, medicinal material solution in contrast, get stachydrine hydrochloride reference substance again to add methyl alcohol and make every 1ml containing the reference substance solution of 1mg, test according to thin-layered chromatography, draw each 10 μ l of above-mentioned solution respectively, put respectively on same silica gel g thin-layer plate, acetone-absolute ethyl alcohol-hydrochloric acid with 10: 6: 1 is for developping agent, launch, take out, dry, put 105 DEG C of heating 5 minutes, spray is with rare bismuth potassium iodide test solution, inspect in the sunlight, in test sample chromatogram, on corresponding to reference substance chromatogram and that control medicinal material chromatogram is corresponding position, the spot of aobvious same color,
(3) assay
Chromatographic condition and system suitability octadecylsilane chemically bonded silica are filling agent; Acetonitrile-1% glacial acetic acid solution with 19: 81 is for mobile phase; Determined wavelength is 323nm; Column temperature 40 DEG C; Flow velocity 0.8ml/min, number of theoretical plate calculates should be not less than 3000 by forulic acid peak,
The preparation of reference substance solution gets forulic acid reference substance in right amount, accurately weighed, adds 50% methyl alcohol and makes the solution of every 1ml containing 10 μ g, to obtain final product,
This product 30 is got in the preparation of need testing solution, and porphyrize, inclines and content, accurately weighed, porphyrize, gets about 4g, accurately weighed, and precision adds methyl alcohol 50ml, weighed weight, ultrasonic process 50 minutes, lets cool, more weighed weight, supply the weight of less loss with methyl alcohol, shake up, filter, accurate absorption subsequent filtrate 15ml, puts in 25ml measuring bottle, is diluted with water to scale, shake up, to obtain final product
Determination method is accurate respectively draws contrast solution and each 20 μ l of need testing solution, injection liquid chromatography, measures, to obtain final product;
Wherein, every described Chanhou Zhuyu Capsule containing Radix Angelicae Sinensis and Ligusticum wallichii with forulic acid (C
10h
10o
4) meter, be no less than 30 μ g.
2. detection method as claimed in claim 1, the power of ultrasonic process in assay process is 120W, and frequency is 59KHz.
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