CN104749261A - A method of examining quality of body resistance-strengthening and detoxifying powder - Google Patents
A method of examining quality of body resistance-strengthening and detoxifying powder Download PDFInfo
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Abstract
The invention relates to a method of examining quality of body resistance-strengthening and detoxifying powder. The method includes examining appearance uniformity of the powder, examining microscopic surface of the powder, detecting granularity of the powder, identifying astragaloside IV in the powder, measuring contents of the astragaloside IV and icariin in the powder, and measuring the water content of the powder. By establishing an identifying method with high specificity, effective examining methods and content measuring methods with good repeatability and good accuracy, the method of examining quality effectively controls the quality of the product, improves quality controllability and stability of the medicine, and ensures safe, effective and stable clinical use of the powder.
Description
Technical field
The invention belongs to Chinese medicine detection technique field, relate to a kind of method checking Fuzheng Jiedu powder quality.
Background technology
Fuzheng Jiedu powder specifies according under " People's Republic of China's veterinary drug allusion quotation " 2010 editions two Fuzheng Jiedu powder items, by the Radix Astragali, Radix Isatidis and barrenwort three taste Chinese medicine combine by a certain percentage pulverize prescribed preparation, there is effect of strengthening vital QI to eliminate pathogenic factors, clearing heat and detoxicating, tonifying middle-Jiao and Qi, cure mainly chicken bursal disease.In addition, also can help to repair immune cell function, induction body produces anti-interferon, reconditioner body immunity function.
In pharmacopeia, under Fuzheng Jiedu powder item, quality standard does not specify discrimination method and the content assaying method of its each effective constituent.The quality standard of " People's Republic of China's veterinary drug allusion quotation " 2010 editions two middle Fuzheng Jiedu powders only has discriminating and check item, does not have assay item.For veterinary drug herbal mixture, the assay of effective constituent needs accurate instrument, and expensive, a lot of veterinary drug producer considers cost, the detecting instrument that seldom configuration is complete, and therefore assay item is often cast out, and Drug's control level is just lower.
Therefore, the quality standard of a perfect Fuzheng Jiedu powder and detection method thereof is needed to set up at present to strengthen quality controllability and the stability of this medicine.
Summary of the invention
Technical matters to be solved by this invention is for the deficiencies in the prior art, provides a kind of method checking Fuzheng Jiedu powder quality.The method comprises quality standard and the method for inspection thereof of Fuzheng Jiedu powder, the method is by setting up the good content assaying method of the strong discrimination method of specificity, effective inspection method and repeatability, accuracy, effectively can control the quality of this product, ensure its Clinical practice safety, effectively, stable.
The method comprises the appearance uniform degree inspecting Fuzheng Jiedu powder, the microcosmic surface inspecting Fuzheng Jiedu powder, the granularity detecting Fuzheng Jiedu powder, the content differentiating Astragaloside IV and icariin in Astragaloside IV in Fuzheng Jiedu powder, detection Fuzheng Jiedu powder and the moisture detected in Fuzheng Jiedu powder.The method, by setting up the good content assaying method of the strong discrimination method of specificity, effective inspection method and repeatability, accuracy, effectively can control the quality of this product, ensure its Clinical practice safety, effectively, stable.
For this reason, the invention provides a kind of method checking Fuzheng Jiedu powder quality, comprise the moisture differentiated Astragaloside IV in Fuzheng Jiedu powder, detect the content of Astragaloside IV and icariin in Fuzheng Jiedu powder and detect in Fuzheng Jiedu powder.
According to the inventive method, differentiate that in Fuzheng Jiedu powder, Astragaloside IV adopts thin-layered chromatography, comprise and compare sample with Astragaloside IV, take methyl alcohol as solvent, with lower floor's solution of the methenyl choloride-methanol-water of 13:7:2 for developping agent, by 2 μ l control sample solution I and Fuzheng Jiedu powder testing sample extract solution I, point sample on same silica gel g thin-layer plate launches respectively, takes out, dries and spray with 10% ethanol solution of sulfuric acid, 105 DEG C to be heated to spot development clear, then inspects; If the result of inspecting is in testing sample chromatogram, on the position corresponding to control sample chromatogram, display and the spot of control sample same color, namely illustrate in testing sample containing Astragaloside IV.
In one embodiment of the invention, the preparation of described testing sample extract solution I comprises: mixed with 20ml methyl alcohol by 8g testing sample and add hot reflux 1 hour, filter, (internal diameter of described alumina column is 10 ~ 15mm obtained filtrate to be added neutral alumina column; The particle diameter of described aluminium oxide is 100 ~ 120 orders, and its consumption is 5g), by the methanol-eluted fractions of 100ml40%, and by eluent evaporate to dryness, institute adds 30ml water in residual residue makes it dissolve, and extracts 2 times, each 20ml with water saturated normal butyl alcohol jolting, merge the n-butanol extracting liquid obtained, wash 2 times with water, each 20ml, n-butanol extracting liquid evaporate to dryness after washing, in residual residue, add 0.5ml methyl alcohol makes it dissolve, and to obtain final product.
In another embodiment of the present invention, described control sample solution I is that solvent obtains with methyl alcohol, and its concentration is 1mg/ml.
According to the inventive method, in described Fuzheng Jiedu powder, the assay of Astragaloside IV adopts high performance liquid chromatography, comprise and adopt evaporative light-scattering detector to detect, and be chromatographic column filling agent with octadecylsilane chemically bonded silica, take Astragaloside IV as control sample, take acetonitrile-water as mobile phase, after reference substance solution II with testing sample extract solution II sample introduction, record chromatogram, the content of Astragaloside IV in Fuzheng Jiedu powder is calculated with external standard two-point method logarithmic equation, wherein, the theoretical cam curve of described chromatographic column calculates by Astragaloside IV peak and is at least 4000.
In one embodiment of the invention, in described mobile phase, the volume ratio of acetonitrile and water is 35:65.The mobile phase of this proportioning can make the chromatographic peak of each composition in testing sample separately, and defects inspecting is clear and definite.
In another embodiment of the present invention, the preparation of described testing sample extract solution II comprises: 10g testing sample is placed in apparatus,Soxhlet's, add 40ml methyl alcohol, cold soaking spends the night, add methyl alcohol again, add hot reflux 4 hours, obtained extract is concentrated into dry, 10ml water is added in residual residue, being heated to 30 ~ 40 DEG C makes it dissolve, 4 times are extracted with water saturated normal butyl alcohol jolting, each 40ml, merge n-butanol extracting liquid, 2 times are washed with the ammonia spirit that concentration is 40vol.%, each about 40ml, by the n-butanol extracting liquid evaporate to dryness after washing, in remaining residue, add 5ml water makes it dissolve, let cool, by D101 type large pore resin absorption column, (internal diameter is 1.5cm, post height is 12cm), first use 50ml water elution, use the ethanol elution of 30ml40% again, use the ethanol elution of 80ml70% again, collect eluent, evaporate to dryness, remaining residue adds methyl alcohol and dissolves and be transferred in 5ml measuring bottle, add methyl alcohol to scale, shake up, obtain.The sample size of described testing sample extract solution II is 10 μ l.
In another embodiment of the present invention, described control sample solution II is that solvent is made with methyl alcohol, and concentration is 0.5mg/ml.The sample size of described control sample solution II is 5 μ l and 15 μ l.
According to the inventive method, in described Fuzheng Jiedu powder, the assay of icariin adopts high performance liquid chromatography, comprise and adopt evaporative light-scattering detector to detect, and be chromatographic column filling agent with octadecylsilane chemically bonded silica, take icariin as control sample, take acetonitrile-water as mobile phase, after reference substance solution III with testing sample extract solution III sample introduction, record chromatogram, the content of icariin in Fuzheng Jiedu powder is calculated with external standard two-point method logarithmic equation, wherein, the theoretical cam curve of described chromatographic column calculates by icariin peak and is at least 1500.
In one embodiment of the invention, in mobile phase, the volume ratio of acetonitrile and water is 25:75.The mobile phase of this proportioning can make the chromatographic peak of each composition in testing sample separately, and defects inspecting is clear and definite.
According to the present invention, the preparation of described testing sample extract solution III comprises testing sample powder is placed in tool plug conical flask, adds ethanol, weighed weight, after ultrasound wave process, more weighed weight, supply the weight of less loss again with ethanol, shake up, elimination impurity and get final product; The sample size of described testing sample extract solution III is 10 μ l.
In one embodiment of the invention, such as, the preparation of described testing sample extract solution III comprises 0.5g testing sample powder is placed in tool plug conical flask, add the ethanol 20ml that concentration is 95%, weighed weight, ultrasound wave process 1 hour, weighed weight again, supply the weight of less loss with the ethanol that concentration is 95%, shake up, elimination impurity and get final product.The sample size of described testing sample extract solution III is 10 μ l.
In another embodiment of the present invention, described control sample solution III is that solvent is made with methyl alcohol, and concentration is 0.1mg/ml.The sample size of described control sample solution III is 5 μ l and 15 μ l.
According to the present invention, described method also comprises the granularity of the appearance uniform degree inspecting Fuzheng Jiedu powder, the microstructure characteristic inspecting Fuzheng Jiedu powder, detection Fuzheng Jiedu powder.Wherein, the appearance uniform degree inspecting Fuzheng Jiedu powder described in comprises and is placed in white smooth flat by testing sample, tiling 5cm
2, its surface is flattened, inspects its color and luster at bright place whether even, whether have decorative pattern and color spot.The granularity of described detection Fuzheng Jiedu powder is that Fuzheng Jiedu powder is crossed 24 mesh sieves, weighs, and calculates the ratio of Fuzheng Jiedu powder by 24 mesh sieves.The described microstructure characteristic inspecting Fuzheng Jiedu powder is interspersed among by Fuzheng Jiedu under microscope to observe.
In the present invention, described Fuzheng Jiedu powder is composed of the following components with parts by weight:
Radix Isatidis 60 parts,
The Radix Astragali 60 parts,
Barrenwort 30 parts;
Wherein, the content calculating Astragaloside IV in described Fuzheng Jiedu powder by dry product is not less than 0.16mg/g; The content calculating icariin in described Fuzheng Jiedu powder by dry product is not less than 0.5mg/g; In described Fuzheng Jiedu powder, liquid water content is not more than 10%(weight), be preferably not more than 6%(weight).
In the present invention, the preparation method of described Fuzheng Jiedu powder is by above 3 kinds of components, pulverizes, sieves, and mixing, to obtain final product.
In the present invention, the particle diameter of described Fuzheng Jiedu powder was that the ratio of the Fuzheng Jiedu scattered seed of 24 mesh sieves is at least 99.2%.Aperture due to 24 mesh sieves is equivalent to 850 ± 29 μm, so the particle diameter of described Fuzheng Jiedu powder is at least 99.2% for the ratio of the Fuzheng Jiedu scattered seed being less than 850 ± 29 μm.
In the present invention, the external appearance characteristic of described Fuzheng Jiedu powder is the powder of lark, and uniform color, without decorative pattern and color spot.
In the present invention, the microstructure characteristic of described Fuzheng Jiedu powder is: fiber bunchy or fall apart from, wall thickness, and there is longitudinal crack on surface, and two ends fragment into broom shape or more truncate; Nonglandular hair 3 ~ 10 cell, long 200 ~ 1000 μm, apical cell is long, and what have is brown or yellowish-brown.
As previously mentioned, in existing pharmacopeia, under Fuzheng Jiedu powder item, quality standard does not specify discrimination method and the content assaying method of its each effective constituent, and its quality standard only has discriminating and check item, does not have assay item.For veterinary drug herbal mixture, the assay of effective constituent needs accurate instrument, and expensive, a lot of veterinary drug producer considers cost, the detecting instrument that seldom configuration is complete, and therefore assay item is often cast out, and Drug's control level is just lower.
In order to improve quality standard and the inspection method thereof of Fuzheng Jiedu powder, better control drug quality, the discrimination method of the present inventor to the composition icariin of barrenwort in Fuzheng Jiedu powder, the composition Astragaloside IV of the Radix Astragali is explored, and determines the content assaying method of icariin and Astragaloside IV in Fuzheng Jiedu powder.
The method of inspection Fuzheng Jiedu powder quality of the present invention comprises the appearance uniform degree inspecting Fuzheng Jiedu powder, the microcosmic surface inspecting Fuzheng Jiedu powder, the granularity detecting Fuzheng Jiedu powder, the content differentiating Astragaloside IV and icariin in Astragaloside IV in Fuzheng Jiedu powder, detection Fuzheng Jiedu powder and the moisture detected in Fuzheng Jiedu powder.The method is by setting up the good content assaying method of the strong discrimination method of specificity, effective inspection method and repeatability, accuracy, effectively can control the quality of this product, quality controllability and the stability of this medicine can be strengthened, ensure its Clinical practice safety, effectively, stablize.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the present invention is described.
Fig. 1 is Radix Astragali qualification thin-layer chromatogram; In figure, Reference numeral is as follows: 1 Astragaloside IV; 2 ~ 4 testing samples; 5 lack Radix Astragali negative control.
Fig. 2 is Astragaloside IV specificity experimental patterns; In figure, the implication of Reference numeral is as follows: 1 Astragaloside IV reference substance chromatogram; 2 testing sample chromatograms; 3 negative control chromatograms.
Fig. 3 is icariin specificity experimental patterns; In figure, the implication of Reference numeral is as follows: 1 icariin reference substance chromatogram; 2 testing sample chromatograms; 3 negative control chromatograms.
Fig. 4 is Astragaloside IV canonical plotting.
Fig. 5 is icariin canonical plotting.
Embodiment
For making the present invention easier to understand, describe the present invention in detail below in conjunction with embodiment and accompanying drawing, these embodiments only play illustrative effect, are not limited to range of application of the present invention, NM specific experiment method in the following example, conveniently experimental technique carries out usually.
Embodiment
Embodiment 1:
1. instrument: Waters e2695 high performance liquid chromatograph; Evaporative light-scattering detector.
Reagent:
Acetonitrile: Tianjin Kermel Chemical Reagent Co., Ltd., chromatographically pure, 20120419.
Methyl alcohol: Chengdu Ke Long chemical reagent factory, chromatographically pure, 20130423.
Normal butyl alcohol: Chengdu Ke Long chemical reagent factory, analyzes pure, and 20110328.
Ammoniacal liquor: Chengdu Ke Long chemical reagent factory, analyzes pure, and 20100419.
Ethanol: Chengdu Ke Long chemical reagent factory, analyzes pure, and 20110703.
Purified water: self-control.
Reference substance:
Astragaloside IV: Nat'l Pharmaceutical & Biological Products Control Institute, content 100%, lot number 110781-200613.
Icariin: Nat'l Pharmaceutical & Biological Products Control Institute, content 100%, lot number 110737-200415.
Sample: Fuzheng Jiedu powder, is produced by Luoyang Huizhong Veterinary Medicine Co. Ltd..
2. the discriminating of Astragaloside IV
The preparation of testing sample extract solution I: 8g testing sample is mixed with 20ml methyl alcohol and adds hot reflux 1 hour, filter, (internal diameter of described alumina column is 10 ~ 15mm obtained filtrate to be added neutral alumina column; The particle diameter of described aluminium oxide is 100 ~ 120 orders, and its consumption is 5g), by the methanol-eluted fractions of 100ml40%, and by eluent evaporate to dryness, institute adds 30ml water in residual residue makes it dissolve, and extracts 2 times, each 20ml with water saturated normal butyl alcohol jolting, merge the n-butanol extracting liquid obtained, wash 2 times with water, each 20ml, n-butanol extracting liquid evaporate to dryness after washing, in residual residue, add 0.5ml methyl alcohol makes it dissolve, and to obtain final product.
The preparation of control sample solution: control sample solution is that solvent obtains with methyl alcohol, and its concentration is 1mg/ml.
Detection method: compare sample with Astragaloside IV, take methyl alcohol as solvent, with lower floor's solution of the methenyl choloride-methanol-water of 13:7:2 for developping agent, by 2 μ l control sample solution and Fuzheng Jiedu powder testing sample extract solution, point sample on same silica gel g thin-layer plate launches respectively, take out, dry and spray with 10% ethanol solution of sulfuric acid, 105 DEG C to be heated to spot development clear, then inspect in testing sample chromatogram, whether the position corresponding to control sample chromatogram shows the spot with control sample same color, inspects and the results are shown in Figure 1.As can be seen from Figure 1, in testing sample chromatogram, whether the position corresponding to control sample chromatogram shows the spot with control sample same color, illustrate in testing sample containing Astragaloside IV.
3. check
Granularity: be 99.2% by the weight of the Fuzheng Jiedu divided powder of 24 mesh sieves.
Appearance uniform degree: get testing sample appropriate, put in glossy paper, tile about 5cm
2, its surface is flattened, observes at bright place, uniform color, without decorative pattern, color spot.
Moisture: measuring according to aquametry (Chinese veterinary pharmacopoeia 2010 editions two annex 60 pages), is 3.2%.
4. assay
Chromatographic condition
Chromatographic column: Kromasil C18 post.
Mobile phase: acetonitrile-water (35:65).
Flow velocity: 1.0ml/min.
Detecting device: evaporative light-scattering detector.
Condition: gas flow 25psi; Gain 150; Drift tube temperature 60 DEG C, sprayer temperature 36 DEG C.
Column temperature: 30 DEG C
1. the preparation of reference substance solution:
It is appropriate that a gets Astragaloside IV reference substance, accurately weighed, adds methyl alcohol and make the solution of every 1ml containing 0.5mg, to obtain final product.
It is appropriate that b gets icariin reference substance, accurately weighed, adds methyl alcohol and make the solution of every 1ml containing 0.1mg, to obtain final product.
2. the preparation of testing sample solution:
A gets this product and is about 10g, accurately weighed, put in apparatus,Soxhlet's, add methyl alcohol 40ml, cold soaking spends the night, add methyl alcohol more appropriate, add hot reflux 4 hours, extract recycling design is also concentrated into dry, residue adds water 10ml, low-grade fever makes dissolving, 4 times are extracted with water saturated normal butyl alcohol jolting, each 40ml, merge normal butyl alcohol liquid, 2 times are fully washed with the ammonia spirit that concentration is 40vol.%, each about 40ml, discard ammoniacal liquor, normal butyl alcohol liquid evaporate to dryness, the residue 5ml that adds water makes dissolving, let cool, by D101 type large pore resin absorption column, (internal diameter is 1.5cm, post height is 12cm), with water 50ml wash-out, discard water liquid, use 40% ethanol 30ml wash-out again, discard eluent, continue with 70% ethanol 80ml wash-out, collect eluent, evaporate to dryness, residue adds methyl alcohol and dissolves, be transferred in 10ml measuring bottle, add methyl alcohol to scale, shake up, obtain.
B gets this product powder and is about 1.0g, accurately weighed, and put in tool plug conical flask, precision adds Diluted Alcohol 20ml, weighed weight, ultrasonic 1 hour, more weighed weight, supplies the weight of less loss, shake up with Diluted Alcohol, filters, gets subsequent filtrate and get final product.
5. specificity test
Take other medicinal material except the Radix Astragali, barrenwort by prescription proportioning and prepare sample as negative sample by preparation technology, getting negative sample and operate with method.Carry out negative sample mensuration, result feminine gender is noiseless simultaneously.Astragaloside IV specificity experimental patterns is shown in Fig. 2, and icariin specificity experimental patterns is shown in Fig. 3.
6. the range of linearity is investigated
Astragaloside IV
Precision takes Astragaloside IV reference substance 25.4mg, adds the solution that methyl alcohol makes 0.508mg/mL, and by above-mentioned chromatographic condition, sample introduction 3 μ L, 5 μ L, 10 μ L, 15 μ L, 20 μ L measure respectively.With peak area logarithm (y) for ordinate, with sample size logarithm (x) for horizontal ordinate, drawing standard curve, obtains regression equation y=1.4828x+5.312, r=0.9991, and in table 1, Astragaloside IV typical curve is shown in Fig. 4.
Table 1 Astragaloside IV linear relationship test findings
| Sample size (μ g) | 1.524 | 2.54 | 5.08 | 7.62 | 10.16 |
| Sample size logarithm | 0.1830 | 0.4048 | 0.7059 | 0.8820 | 1.0069 |
| Peak area | 363293 | 876641 | 2334700 | 3999771 | 6394317 |
| Peak area logarithm | 5.5603 | 5.9428 | 6.3682 | 6.6020 | 6.8058 |
Above result shows, within the scope of 1.524 μ g ~ 10.16 μ g, peak area logarithm and sample size logarithm have good linear relationship.
Icariin
Precision takes icariin reference substance 24.8mg, adds the solution that methyl alcohol makes 0.1048mg/mL, and by above-mentioned chromatographic condition, sample introduction 3 μ L, 5 μ L, 10 μ L, 15 μ L, 20 μ L measure respectively.With peak area logarithm (y) for ordinate, with sample size logarithm (x) for horizontal ordinate, drawing standard curve, obtains regression equation y=0.9788x+6.5227, r=0.9992, in table 2.Icariin typical curve is shown in Fig. 5.
Table 2 icariin linear relationship test findings
| Sample size (μ g) | 0.3144 | 0.5240 | 1.0480 | 1.5720 | 2.0960 |
| Sample size logarithm | -0.5025 | -0.2807 | -0.02036 | 0.1965 | 0.3214 |
| Peak area | 1057258 | 1760252 | 3357768 | 5085679 | 6786428 |
| Peak area logarithm | 6.0242 | 6.2456 | 6.5261 | 6.7063 | 6.8316 |
Above result shows, within the scope of 0.3144 μ g ~ 2.0960 μ g, peak area logarithm and sample size logarithm have good linear relationship.
7. precision test
Accurate absorption Astragaloside IV reference substance solution (0.508mg/ml) 10 μ l, repeat sample introduction 6 times, the RSD=1.27% of Astragaloside IV peak value, the results are shown in Table 3.
Table 3 Astragaloside IV Precision test result
| Test number (TN) | 1 | 2 | 3 | 4 | 5 | 6 | On average |
| Peak area | 2334700 | 2371256 | 2302154 | 2346253 | 2312365 | 2292659 | 2326565 |
Accurate absorption icariin reference substance solution (0.1048mg/mL) 10 μ l, repeat sample introduction 6 times, the RSD=1.04% of icariin peak value, the results are shown in Table 4.
Table 4 icariin Precision test result
| Test number (TN) | 1 | 2 | 3 | 4 | 5 | 6 | On average |
| Peak area | 2555636 | 2546174 | 2536002 | 2588071 | 2507306 | 2555636 | 2548138 |
8. stability test
Sample thief prepares testing sample solution by the Determination of Astragaloside method drafted, and measures respectively at 0,2,4,8,12,24 hour.Measurement result calculates RSD% with Astragaloside content, the results are shown in Table 5.
Table 5 Astragaloside IV stability test result
| Minute (h) | 0 | 2 | 4 | 8 | 12 | 24 | On average | RSD% |
| Content (mg/g) | 0.183 | 0.181 | 0.189 | 0.179 | 0.182 | 0.188 | 0.184 | 2.2 |
Sample thief prepares testing sample solution by the Determination of Content of Icariin method drafted, and measures respectively at 0,2,4,8,12,24 hour.Measurement result calculates RSD% with Icariin content, the results are shown in Table 6.
Table 6 icariin stability test result
| Minute (h) | 0 | 2 | 4 | 8 | 12 | 24 | On average | RSD% |
| Content (mg/g) | 0.75 | 0.71 | 0.75 | 0.73 | 0.73 | 0.72 | 0.73 | 2.2 |
Test findings shows, the Astragaloside IV in testing sample solution and icariin good at 24 hours internal stabilities.
9. replica test
Get same batch sample and prepare testing sample solution by the Determination of Astragaloside method drafted, prepare 6 parts respectively for mensuration.Measurement result calculates RSD% with Astragaloside content, the results are shown in Table 7.
Table 7 Astragaloside IV replica test result
| Measure number of times | 1 | 2 | 3 | 4 | 5 | 6 | On average | RSD% |
| Content (mg/g) | 0.183 | 0.186 | 0.179 | 0.176 | 0.182 | 0.186 | 0.182 | 2.2 |
Get same batch sample and prepare testing sample solution by the Determination of Content of Icariin method drafted, prepare 6 parts respectively for mensuration.Measurement result, to calculate RSD% with Icariin content, the results are shown in Table 8.
Table 8 icariin replica test result
| Minute (h) | 1 | 2 | 3 | 4 | 5 | 6 | On average | RSD% |
| Content (mg/g) | 0.73 | 0.72 | 0.74 | 0.68 | 0.72 | 0.71 | 0.72 | 2.9 |
Test findings shows, the Astragaloside IV in testing sample solution and icariin repeatability are well.
10. recovery test
Get 6 parts, the sample of known content, every part of 5.0g, accurately weighed, put in tool plug conical flask, each precision adds the Astragaloside IV reference substance methanol solution 2mL of 0.508mg/mL, by the content assaying method drafting Astragaloside IV, prepare testing sample solution, measure peak area and calculate content, calculating the recovery, the results are shown in Table 9.
Table 9 Astragaloside IV recovery test result
Test findings shows: the recovery is between 95% ~ 105%, average 101.85%, RSD%=2.8<5.0, and average recovery conforms with the regulations.
Get 6 parts, the sample of known content, every part of 0.5g, accurately weighed, put in tool plug conical flask, each precision adds the icariin reference substance methanol solution 5mL of 0.1048mg/mL, by the content assaying method drafting icariin, prepare testing sample solution, measure peak area and calculate content, calculating the recovery, the results are shown in Table 10.
Table 10 icariin recovery test result
Test findings shows: the recovery is between 95% ~ 105%, average 100.23%, RSD%=2.6<5.0, and average recovery conforms with the regulations.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. check a method for Fuzheng Jiedu powder quality, comprise the moisture differentiated Astragaloside IV in Fuzheng Jiedu powder, detect the content of Astragaloside IV and icariin in Fuzheng Jiedu powder and detect in Fuzheng Jiedu powder.
2. method according to claim 1, it is characterized in that, in described Fuzheng Jiedu powder, the assay of icariin adopts high performance liquid chromatography, comprise and adopt evaporative light-scattering detector to detect, and be chromatographic column filling agent with octadecylsilane chemically bonded silica, take icariin as control sample, take acetonitrile-water as mobile phase, after reference substance solution III with testing sample extract solution III sample introduction, record chromatogram, the content of icariin in Fuzheng Jiedu powder is calculated with external standard two-point method logarithmic equation, wherein, the theoretical cam curve of described chromatographic column calculates by icariin peak and is at least 1500.
3. method according to claim 2, is characterized in that, in mobile phase, the volume ratio of acetonitrile and water is 25:75.
4. according to the method in claim 2 or 3, it is characterized in that, the preparation of described testing sample extract solution III comprises testing sample powder is placed in tool plug conical flask, add ethanol, weighed weight, after ultrasound wave process, weighed weight again, supply the weight of less loss again with ethanol, shake up, elimination impurity and get final product; The sample size of described testing sample extract solution III is 10 μ l.
5. according to the method in claim 2 or 3, it is characterized in that, described control sample solution III is that solvent is made with methyl alcohol, and concentration is 0.1mg/ml; The sample size of described control sample solution III is 5 μ l and 15 μ l.
6. method according to claim 1, it is characterized in that, in described Fuzheng Jiedu powder, the assay of Astragaloside IV adopts high performance liquid chromatography, comprise and adopt evaporative light-scattering detector to detect, and be chromatographic column filling agent with octadecylsilane chemically bonded silica, take Astragaloside IV as control sample, take acetonitrile-water as mobile phase, after reference substance solution II with testing sample extract solution II sample introduction, record chromatogram, the content of Astragaloside IV in Fuzheng Jiedu powder is calculated with external standard two-point method logarithmic equation, wherein, the theoretical cam curve of described chromatographic column calculates by Astragaloside IV peak and is at least 4000.
7. method according to claim 6, is characterized in that, in described mobile phase, the ratio of acetonitrile and water is 35:65.
8. according to the method in claim 1 to 7 described in any one, it is characterized in that, described method also comprises the granularity of the appearance uniform degree inspecting Fuzheng Jiedu powder, the microstructure characteristic inspecting Fuzheng Jiedu powder, detection Fuzheng Jiedu powder;
Wherein, the appearance uniform degree inspecting Fuzheng Jiedu powder described in comprises and is placed in white smooth flat by testing sample, tiling 5cm
2, its surface is flattened, inspects its color and luster at bright place whether even, whether have decorative pattern and color spot;
The granularity of described detection Fuzheng Jiedu powder is that Fuzheng Jiedu powder is crossed 24 mesh sieves, weighs, and calculates the ratio of Fuzheng Jiedu powder by 24 mesh sieves;
The described microstructure characteristic inspecting Fuzheng Jiedu powder is interspersed among by Fuzheng Jiedu under microscope to observe.
9. according to the method in claim 1 to 8 described in any one, it is characterized in that, described Fuzheng Jiedu powder is composed of the following components with parts by weight:
Radix Isatidis 60 parts,
The Radix Astragali 60 parts,
Barrenwort 30 parts;
Wherein, the content calculating Astragaloside IV in described Fuzheng Jiedu powder by dry product is not less than 0.16mg/g; The content calculating icariin in described Fuzheng Jiedu powder by dry product is not less than 0.5mg/g; In described Fuzheng Jiedu powder, liquid water content is not more than 10%(weight), be preferably not more than 6%(weight).
10. method according to claim 9, is characterized in that,
The particle diameter of described Fuzheng Jiedu powder was that the ratio of the Fuzheng Jiedu scattered seed of 24 mesh sieves is at least 99.2%;
The external appearance characteristic of described Fuzheng Jiedu powder is the powder of lark, and uniform color, without decorative pattern and color spot;
The microstructure characteristic of described Fuzheng Jiedu powder is: fiber bunchy or fall apart from, wall thickness, and there is longitudinal crack on surface, and two ends fragment into broom shape or more truncate; Nonglandular hair 3 ~ 10 cell, long 200 ~ 1000 μm, apical cell is long, and what have is brown or yellowish-brown.
Priority Applications (1)
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| CN108061762A (en) * | 2017-03-06 | 2018-05-22 | 石家庄平安医院有限公司 | The content assaying method of three kinds of flavone components in a kind of kidney tonifying eliminating toxic particle |
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| CN108061762A (en) * | 2017-03-06 | 2018-05-22 | 石家庄平安医院有限公司 | The content assaying method of three kinds of flavone components in a kind of kidney tonifying eliminating toxic particle |
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