CN103543214A - Determination method of content of active ingredient of Pingxiao capsule - Google Patents
Determination method of content of active ingredient of Pingxiao capsule Download PDFInfo
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Abstract
The invention relates to a determination method of the content of an active ingredient of a Pingxiao capsule. The determination method includes preparation of a reference solution, preparation of a test solution and formulation of high performance liquid chromatography conditions, wherein naringin content is not less than 2.13mg/particle and neohesperidin content is not less than 1.22mg/particle. The determination method is simple, safe and reliable, and is capable of faithfully representing product content and quality; the determination method is suitable for industrial daily production and inspection.
Description
Technical field
The present invention relates to field of medicaments, especially relate to the content assaying method of PING XIAO JIAO NANG effective constituent.
Background technology
Existing Chinese patent drug PING XIAO JIAO NANG is a kind of conventional antineoplastic Chinese traditional medicine.[assay] of the PING XIAO JIAO NANG of recording in pharmacopeia and ministerial standard gets 30 of this product, pour out content, accurately weighed, porphyrize, get the about 4g of powder, accurately weighed, put in 100ml tool plug conical flask, precision adds chloroform 20ml and liquor ammoniae fortis 1ml, close plug, weighed weight, cold soaking 48 hours, or ultrasonic extraction 40 minutes, weigh, with chloroform, supply the weight of loss, shake well, filter, precision measures filtrate 10ml, put in separating funnel, with sulfuric acid solution (0.5mol/L), extract 4 times, each 10ml, extract all with sulfuric acid solution (0.5mol/L) in advance moistening filter paper filter in 50ml measuring bottle, and with the appropriate washing nozzle of sulfuric acid solution (0.5mol/L), washing lotion is incorporated in measuring bottle, add again sulfuric acid solution (0.5mol/L) to scale, shake up, precision measures 10ml, put in 50ml measuring bottle, add sulfuric acid liquid (0.5mol/L) to scale, shake up according to spectrophotometric method, at 262nm and 300nm wavelength place, measure absorbance log, every of heavy this product of average particle contains vomiting nut in strychnine (C12H22N2O2), should be 0.25～0.35mg.
PING XIAO JIAO NANG prescription is root tuber of aromatic turmeric 54g hairyvein agrimony 54g excrementum pteropi 45g alum 54g nitre 54g dried lacquer (system) 18g Fructus Aurantii (bran stir-fry) 90g prepared nux vomica 36g, the content of Fructus Aurantii is maximum, it is topmost component, in above-mentioned pharmacopeia, content assaying method is only measured the content of strychnine in vomiting nut, the quality that can not truly reflect product, to such an extent as to the stability of product is uncontrollable, bring hidden danger to production and patient.
Summary of the invention
In order to solve the problems of the technologies described above, the invention provides a kind of content assaying method of PING XIAO JIAO NANG effective constituent, the method accurately, reliable, the quality that can truly reflect product.
The present invention is achieved by the following technical solutions:
In PING XIAO JIAO NANG, a content assaying method for effective constituent, comprises the steps:
(1) preparation of reference substance: get aurantiin, neohesperidin reference substance is appropriate;
(2) preparation of test sample: make even capsule for eliminating content with after methyl alcohol or alcohol extract as for standby in volumetric flask;
(3) high-efficient liquid phase chromatogram condition: C
184.6 * 250mm, 5 μ m chromatographic columns, mobile phase acetonitrile-water, flow velocity 0.5-1.2mlmin
-1detect wavelength 245-360nm;
(4) determination method: precision is drawn reference substance and need testing solution injection liquid chromatography and be get final product.
The described aurantiin reference substance of above-mentioned steps (1) concentration is 80ug/1ml, neohesperidin reference substance concentration 60ug/1ml.
Test sample described in above-mentioned steps (2) with after the ultrasonic extraction of methyl alcohol as for standby in volumetric flask.Test sample described in preferred steps (2) adds methyl alcohol 25ml, weighed weight, ultrasonic processing 30 minutes, let cool, more weighed weight, with methyl alcohol, supply the weight of less loss, shake up, filter, discard just filtrate, precision measures subsequent filtrate 5ml, put in 25ml measuring bottle, with methyl alcohol, be diluted to scale, shake up, obtain.
In above-mentioned steps (3), the pH value of mobile phase is 2.0-5.0, mobile phase acetonitrile-water 15-30: mobile phase acid for adjusting pH value described in 85-70., is preferably pH value 3.0, mobile phase acetonitrile-water=20: 80; Described acid includes but not limited to as phosphoric acid, acetic acid, formic acid, citric acid, tartrate, hydrogen sulfate are received, potassium acid sulfate, hydrochloric acid, sulfuric acid, carbonic acid, perchloric acid, malic acid, citric acid, salicylic acid, caffeic acid etc., preferably phosphoric acid, acetic acid, formic acid, citric acid, tartrate, hydrogen sulfate are received, potassium acid sulfate etc., and the best is phosphoric acid.Described phosphoric acid concentration is 5-20%, and preferred concentration is 10%.In the present invention, preferably 10% phosphoric acid can make each chromatographic peak in PING XIAO JIAO NANG have good separation, improves peak conditions of streaking.
Preferred flow phase acetonitrile-water=20 described in above-mentioned steps (3): 80, flow velocity is 1.0mlmin
-1, detect wavelength 283nm
Described in above-mentioned steps (4), measure, preferably naringin content is not less than 2.26mg/ grain, and neohesperidin content is not less than 1.33mg/ grain.
The PING XIAO JIAO NANG active constituent content measuring method of the best of the present invention, comprises the steps:
(1) preparation of reference substance: it is appropriate that precision takes aurantiin reference substance, adds methyl alcohol and makes every 1ml containing the solution of aurantiin 80ug; It is appropriate that precision takes neohesperidin reference substance, adds methyl alcohol and make every 1ml containing the solution of neohesperidin 60ug;
(2) get 20 of capsules, put porphyrize in mortar and cross sieve No. four, get about 0.5g, accurately weighed, put in tool plug conical flask, precision adds methyl alcohol 25ml, weighed weight, ultrasonic processing 30 minutes, lets cool, more weighed weight, the weight of supplying less loss with methyl alcohol, shakes up, and filters, discard just filtrate, precision measures subsequent filtrate 5ml, puts in 25ml measuring bottle, with methyl alcohol, be diluted to scale, shake up, obtain;
(3) high-efficient liquid phase chromatogram condition
Chromatographic column: WatersC
18post 4.6 * 250mm, 5 μ m, mobile phase: acetonitrile-water=20: 80, with 10% phosphoric acid regulating ph value 3.0; Detection wavelength is 283nm; Column temperature: room temperature; Flow velocity: 1.0mlmin
-1; Input mode: auto injection;
(4) accurate reference substance solution and each 10 μ l of need testing solution of drawing of determination method difference, injection liquid chromatography, measures, and obtains.
The prescription of PING XIAO JIAO NANG of the present invention is: weight portion medicinal material root tuber of aromatic turmeric 1-5 part, hairyvein agrimony 1-5 part, excrementum pteropi 1-5 part, alum 1-5, nitre 1-5, dried lacquer 0.5-3 part processed, stir-baked FRUCTUS AURANTII in bran 3-7 part, prepared nux vomica 0.5-4 part.Preferred weight part medicinal material root tuber of aromatic turmeric 2-4 part, hairyvein agrimony 2-4 part, excrementum pteropi 2-4 part, alum 2-4, nitre 2-4 part, dried lacquer 0.5-2 part processed, stir-baked FRUCTUS AURANTII in bran 4-6 part, prepared nux vomica 1-3 part.3 parts of optimum weight part medicinal material root tubers of aromatic turmeric, 3 parts of hairyvein agrimonies, 2.5 parts of excrementum pteropis, 3 parts of alums, 3 parts, nitre, 1 part of dried lacquer processed, 5 parts of stir-baked FRUCTUS AURANTII in bran, 2 parts of prepared nux vomicas.
The preparation method of PING XIAO JIAO NANG of the present invention is prepared according to pharmacopeia, preferred following method preparation:
Above 8 taste medicinal materials, get dried lacquer, excrementum pteropi, alum, nitre and are ground into fine powder, get root tuber of aromatic turmeric, stir-baked FRUCTUS AURANTII in bran is pulverized, and with ethanol, is that solvent carries out diacolation, collection percolate; The dregs of a decoction after diacolation and hairyvein agrimony boiling secondary, filter collecting decoction; Percolate reclaims after ethanol, merges with above-mentioned filtrate, and reduced pressure concentration becomes thick paste, dry, pulverize into fine powder, adds prepared nux vomica, above-mentioned fine powder and right amount of auxiliary materials, mixes, and granulates, dry, incapsulates, and obtains.
Best, preparation method of the present invention, comprises the steps:
Above eight tastes, dried lacquer, excrementum pteropi, alum, nitre are ground into fine powder; Root tuber of aromatic turmeric, stir-baked FRUCTUS AURANTII in bran are ground into meal, with 70% ethanol, are solvent, carry out diacolation, collect percolate; The dregs of a decoction and hairyvein agrimony boiling secondary, filter collecting decoction; Percolate reclaims after ethanol, merges with above-mentioned filtrate, and reduced pressure concentration becomes thick paste, dry, pulverize into fine powder, adds prepared nux vomica, above-mentioned fine powder and right amount of auxiliary materials, mixes, and granulates, dry, incapsulates, and obtains.
In order better to prove the safe and reliable of assay of the present invention, the present invention is verified by following methodology.
The checking of test example methodology
1 instrument and reagent
Reagent: acetonitrile (chromatographically pure), methyl alcohol, phosphoric acid are analysis alcohol.
Sample: Xi'an Zhengda Pharmaceutical Co., Ltd. provides.
Reference substance: aurantiin reference substance (lot number: 110722-200309), neohesperidin reference substance (lot number: 111857-201001) provide by Nat'l Pharmaceutical & Biological Products Control Institute, for assay.
Instrument: high performance liquid chromatograph (Agilent1200); ; DELTA 320 PH meters (plum Teller-Tuo benefit Instrument Ltd.); AL-204 type electronic analytical balance (Max=210g, d=0.0001g, plum Teller-Tuo benefit Instrument Ltd.); TG332A type micro-analytical balance (Max=20g, d=0.01mg); HQ-500DE type ultrasonic cleaner (Kunshan Ultrasonic Instruments Co., Ltd.).
2, chromatographic condition: see embodiment mono-
3, reference substance solution preparation: see embodiment mono-
4, need testing solution preparation: see embodiment mono-
5, lack the preparation of the negative need testing solution of Fructus Aurantii
By prescription, form 1/10th deals, get remove Fructus Aurantii all the other flavour of a drug together, by technological requirement, make not containing the negative sample of Fructus Aurantii, get this negative sample, by the preparation method of need testing solution, prepare the negative need testing solution that lacks Fructus Aurantii.
6, determination method: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and injection liquid chromatography, measures, and obtains.
7, the negative sample interference that lacks Fructus Aurantii is measured:
Precision is drawn above-mentioned reference substance solution respectively, each 10 μ l of the negative need testing solution of need testing solution and scarce Fructus Aurantii, injection liquid chromatography, measure, need testing solution is existing together mutually and is having corresponding chromatographic peak with reference substance solution retention time, and the negative need testing solution that lacks Fructus Aurantii is existing together mutually and there is no corresponding chromatographic peak with reference substance solution retention time, but consistent with other chromatographic peak retention time of need testing solution, chromatographic peak abundant information, negative sample is noiseless.
8, the investigation of linear relationship
(concentration is respectively accurate absorption aurantiin reference substance solution respectively, every 1ml is containing aurantiin 8.48ug, 25.44ug, 42.4ug, 59.36ug, 84.8ug) each 10ul, (concentration is respectively neohesperidin reference substance solution, every 1ml is containing neohesperidin 7.95ug, 23.85ug, 39.75ug, 55.65ug, 79.5ug) each 10ul, injection liquid chromatography, measures respectively.Take reference substance concentration as horizontal ordinate (X), take peak area as ordinate (Y) carries out linear regression, obtain aurantiin and neohesperidin equation of linear regression.The aurantiin range of linearity is good linear relationship within the scope of 8.48～84.8 μ g.Equation of linear regression is Y=15.819X-3.3008; R2=0.9999.Result is respectively in Table 1 and Fig. 1.The neohesperidin range of linearity is good linear relationship within the scope of 7.95～79.5 μ g.Equation of linear regression is Y=17.518X-1.9234; R2=1.Result is respectively in Table 2 and Fig. 2.
Table 1 aurantiin linear relationship is investigated result
| Sequence number | Aurantiin concentration | Peak |
| 1 | 8.48μg | 133.2 |
| 2 | 25.44μg | 397.1 |
| 3 | 42.40μg | 671.4 |
| 4 | 59.36μg | 926.8 |
| 5 | 84.80μg | 1342.8 |
Table 2 neohesperidin linear relationship is investigated result
| Sequence number | Neohesperidin concentration | |
| 1 | 7.95μg | 138 |
| 2 | 23.85μg | 418.2 |
| 3 | 39.75μg | 690.8 |
| 4 | 55.65μg | 971.65 |
| 5 | 79.50μg | 1392.75 |
9, precision test
The capsule for eliminating need testing solution of making even, by above-mentioned chromatographic condition, repeats respectively sample introduction 6 times, and result of calculation, respectively in Table 3
Table 3 PING XIAO JIAO NANG precision result
From above result, this instrument precision is good.
10, stability test
At ambient temperature, PING XIAO JIAO NANG need testing solution (110118k criticizes), by " need testing solution " method, prepare test sample, respectively at preparation after 0,2,4,6,8,10,12,14,16,18,20,22, the 24h time interval, aurantiin, neohesperidin content in difference working sample, and calculate its RSD value.The results are shown in Table 4.
The stability test of table 4 PING XIAO JIAO NANG
Result shows, at room temperature, within 24 hours, internal stability is good for need testing solution.
11, reappearance test
Six parts of PING XIAO JIAO NANGs (110118k criticizes) getting respectively same lot number, the preparation method who presses need testing solution, prepares 6 parts of need testing solutions, by above-mentioned chromatographic condition, measures respectively, calculates its content.The results are shown in Table 5.
The test of table 5 PING XIAO JIAO NANG reappearance
Result shows that the method reappearance is good.
12 recovery tests
Accurate PING XIAO JIAO NANG (110118k criticizes) sample that takes known content is 6 parts respectively, according to appendix X VIII A traditional Chinese medicine quality standard method of analysis verification guide principle of < < Chinese Pharmacopoeia > > version in 2010, accurately weighed aurantiin reference substance, neohesperidin reference substance are appropriate, put in 200ml volumetric flask, add methyl alcohol and dissolve and be settled to scale.Precision is drawn certain density aurantiin reference substance solution (0.2727mg/ml) 10ml respectively, add in accurately weighed sample, from " putting tool plug conical flask; precision adds methyl alcohol 10ml ", rise, to " precision measures subsequent filtrate 5ml, puts in 25ml measuring bottle, is diluted to scale; shake up with methyl alcohol, obtains." prepare need testing solution.Accurate certain density neohesperidin reference substance solution (0.1568mg/ml) 10ml that draws adds in accurately weighed sample again, from " putting tool plug conical flask; precision adds methyl alcohol 10ml ", rise, to " precision measures subsequent filtrate 5ml; put in 25ml measuring bottle; be diluted to scale with methyl alcohol, shake up, obtain." prepare need testing solution.The method worked out by text is measured content, with following formula calculate recovery rate, result respectively in Table 6, table 7.
Computing formula:
Reference substance addition (mg)
Table 6 PING XIAO JIAO NANG aurantiin average recovery result
Table 7 PING XIAO JIAO NANG neohesperidin average recovery result
From above-mentioned table 6,7 recovery, this method is safe and reliable, can truly reflect product content.
130 batch sample assay results
The PING XIAO JIAO NANG sample of getting ten lot numbers, the content assaying method of working out according to text is prepared respectively need testing solution, by above-mentioned chromatographic condition, analyzes, and the results are shown in Table 8.
Ten batches of PING XIAO JIAO NANG assay results of table 8
| Lot number | Naringin content (mg/ grain) | Neohesperidin content (mg/ grain) |
| 1011129 | 2.92 | 1.71 |
| 1011131 | 3.27 | 1.92 |
| 1011133 | 3.26 | 1.91 |
| 1012135 | 3.19 | 1.88 |
| 1012137 | 2.99 | 1.76 |
| 1012140 | 2.99 | 1.76 |
| 1101155k | 3.14 | 1.76 |
| 1101160k | 2.95 | 1.67 |
| 1101161k | 2.72 | 1.47 |
| 1101162k | 2.97 | 1.57 |
| Average content | 3.04 | 1.74 |
According to 10 batches of PING XIAO JIAO NANG assay results and rate of transform influence factor, limit is decided to be:
Aurantiin: 3.04mg/ grain * 70%=2.13mg/ grain,
Neohesperidin: 1.74mg/ grain * 70%=1.22mg/ grain
In sum, the content assaying method of PING XIAO JIAO NANG of the present invention is simple, reliable, strong operability, suitable daily production testing.Chromatographic peak degree of separation of the present invention is high.Completely separated, act charitably in peak, and without tailed peak and leading peak, impurity peaks undopes in each chromatographic peak.
Accompanying drawing explanation
Fig. 1 aurantiin linear relationship chart
Fig. 2 neohesperidin linear relationship chart
Embodiment
By embodiment below, explaining content of the present invention, is not the further restriction to protection domain of the present invention.
Get 54 grams of weight portion medicinal material root tubers of aromatic turmeric, 54 grams of hairyvein agrimonies, 45 grams of excrementum pteropis, 54 grams of alums, 54 grams, nitre, 18 grams of dried lacquers processed, 90 grams of stir-baked FRUCTUS AURANTII in bran, 36 grams of prepared nux vomicas; Above eight tastes, dried lacquer, excrementum pteropi, alum, nitre are ground into fine powder; Root tuber of aromatic turmeric, stir-baked FRUCTUS AURANTII in bran are ground into meal, with 70% ethanol, are solvent, carry out diacolation, collect percolate 600ml, reclaim ethanol, standby; The dregs of a decoction and hairyvein agrimony boiling secondary, filter, and merging filtrate also merges with above-mentioned percolate, and reduced pressure concentration becomes thick paste, dry, adds prepared nux vomica, above-mentioned fine powder and starch appropriate, mixes, and granulates, dry, incapsulates, and makes 1000, obtains.
Content assaying method
(1) preparation of reference substance: it is appropriate that precision takes aurantiin reference substance, adds methyl alcohol and makes every 1ml containing the solution of aurantiin 80ug; It is appropriate that precision takes neohesperidin reference substance, adds methyl alcohol and make every 1ml containing the solution of neohesperidin 60ug
(2) get 20 of this product, put porphyrize in mortar and cross sieve No. four, get about 0.5g, accurately weighed, put in tool plug conical flask, precision adds methyl alcohol 25ml, weighed weight, ultrasonic processing 30 minutes, lets cool, more weighed weight, the weight of supplying less loss with methyl alcohol, shakes up, and filters, discard just filtrate, precision measures subsequent filtrate 5ml, puts in 25ml measuring bottle, with methyl alcohol, be diluted to scale, shake up, obtain.
(3) high-efficient liquid phase chromatogram condition
Chromatographic column: WatersC
18post 4.6 * 250mm, 5 μ m, mobile phase: acetonitrile-water=20: 80, with 10% phosphorus acid for adjusting pH value 3.0; Detection wavelength is 283nm; Column temperature: room temperature; Flow velocity: 1.0mlmin
-1; Input mode: auto injection.
(4) accurate reference substance solution and each 10 μ l of need testing solution of drawing of determination method difference, injection liquid chromatography, measures naringin content 3.04mg/ grain, neohesperidin content 1.74mg/ grain.
Embodiment 2
Reference substance solution is according to embodiment 1 preparation
Need testing solution: get 20 of the PING XIAO JIAO NANGs of embodiment 1, put porphyrize in mortar and cross sieve No. four, get about 0.5g, accurately weighed, to put in tool plug conical flask, precision adds ethanol 25ml refluxing extraction to process 30 minutes, let cool, filter, reduced pressure concentration is dry, after dissolving with 25ml methyl alcohol, constant volume is in 25ml volumetric flask again, precision measures subsequent filtrate 5ml, puts in 25ml measuring bottle, with methyl alcohol, is diluted to scale, shake up, obtain.
Chromatographic condition: WatersC
18post 4.6 * 250mm, 5 μ m, mobile phase: acetonitrile-water=15: 85, with 20% phosphorus acid for adjusting pH value 2.0; Detection wavelength is 283nm; Column temperature: room temperature; Flow velocity: 1.2mlmin
-1; Input mode: auto injection.
Determination method is accurate reference substance solution and each 10 μ l of need testing solution of drawing respectively, and injection liquid chromatography, measures naringin content 2.99mg/ grain, neohesperidin content 1.67mg/ grain.
Embodiment 3
Reference substance solution is according to embodiment 1 preparation
Need testing solution: get 20 of the PING XIAO JIAO NANGs of embodiment 1, put porphyrize in mortar and cross sieve No. four, get about 0.5g, accurately weighed, put in tool plug conical flask, precision adds methyl alcohol 25ml, weighed weight, ultrasonic processing 40 minutes, lets cool, more weighed weight, the weight of supplying less loss with methyl alcohol, shakes up, and filters, discard just filtrate, precision measures subsequent filtrate 5ml, puts in 25ml measuring bottle, with methyl alcohol, be diluted to scale, shake up, obtain.
Chromatographic condition: WatersC
18post 4.6 * 250mm, 5 μ m, mobile phase: acetonitrile-water=30: 70, with 5% phosphoric acid regulating ph value 5.0; Detection wavelength is 283nm; Column temperature: room temperature; Flow velocity: 0.5mlmin
-1; Input mode: auto injection.
Determination method is accurate reference substance solution and each 10 μ l of need testing solution of drawing respectively, and injection liquid chromatography, measures naringin content 2.99mg/ grain, neohesperidin content 1.76mg/ grain.
Claims (10)
1. a content assaying method for effective constituent in PING XIAO JIAO NANG, is characterized in that, comprises the steps:
(1) preparation of reference substance: get aurantiin, neohesperidin reference substance is appropriate;
(2) preparation of test sample: the capsule for eliminating sample contents of making even with after methyl alcohol or alcohol extract as for standby in volumetric flask;
(3) high-efficient liquid phase chromatogram condition: C
184.6 * 250mm, 5 μ m chromatographic columns, mobile phase acetonitrile-water, flow velocity 0.5-1.2mlmin
-1detect wavelength 245-360nm;
(4) determination method: precision is drawn reference substance and need testing solution injection liquid chromatography and be get final product.
2. content assaying method as claimed in claim 1, is characterized in that: in described step (1), aurantiin reference substance concentration is 80ug/1ml, neohesperidin reference substance concentration 60ug/1ml.
3. content assaying method as claimed in claim 1, is characterized in that: the test sample described in step (2) with after the ultrasonic extraction of methyl alcohol as for standby in volumetric flask.
4. content assaying method as claimed in claim 3, is characterized in that: the test sample described in step (2) adds methyl alcohol 25ml, weighed weight, ultrasonic processing 30 minutes, lets cool, more weighed weight, the weight of supplying less loss with methyl alcohol, shakes up, and filters, discard just filtrate, precision measures subsequent filtrate 5ml, puts in 25ml measuring bottle, with methyl alcohol, is diluted to scale, shake up, obtain.
5. content assaying method as claimed in claim 1, is characterized in that: in described step (3), the pH value of mobile phase is 2.0-5.0, mobile phase acetonitrile-water=15-30: 85-70.
6. content assaying method as claimed in claim 4, it is characterized in that: mobile phase acid for adjusting pH value is 3.0 in described step (3), described acid is that phosphoric acid, acetic acid, formic acid, citric acid, tartrate, hydrogen sulfate are received, a kind of in potassium acid sulfate.
7. content assaying method as claimed in claim 5, is characterized in that: in described step (3), acid is phosphoric acid, and concentration is 5-20%.
8. content assaying method as described in claim 1 or 5, is characterized in that: mobile phase acetonitrile-water=20 described in step (3): 80, and flow velocity is 1.0mlmin
-1, detect wavelength 283nm.
9. content assaying method as claimed in claim 1, is characterized in that: described in step (4), measure, naringin content is not less than 2.13mg/ grain, and neohesperidin content is not less than 1.22mg/ grain.
10. content assaying method as claimed in claim 1, its feature exists, and comprises the steps:
(1) preparation of reference substance: it is appropriate that precision takes aurantiin reference substance, adds methyl alcohol and makes every 1ml containing the solution of aurantiin 80ug;
It is appropriate that precision takes neohesperidin reference substance, adds methyl alcohol and make every 1ml containing the solution of neohesperidin 60ug;
(2) preparation of test sample: 20 of the capsule for eliminating of making even, put porphyrize in mortar and cross sieve No. four, get about 0.5g, accurately weighed, put in tool plug conical flask, precision adds methyl alcohol 25ml, weighed weight, ultrasonic processing 30 minutes, lets cool, more weighed weight, the weight of supplying less loss with methyl alcohol, shakes up, and filters, discard just filtrate, precision measures subsequent filtrate 5ml, puts in 25ml measuring bottle, with methyl alcohol, be diluted to scale, shake up, obtain;
(3) high-efficient liquid phase chromatogram condition
Chromatographic column: Waters C
18post 4.6 * 250mm, 5 μ m, mobile phase: acetonitrile-water=20: 80, with 10% phosphoric acid regulating ph value 3.0; Detection wavelength is 283nm; Column temperature: room temperature; Flow velocity: 1.0mlmin
-1; Input mode: auto injection;
(4) determination method: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and injection liquid chromatography, measures, and obtains.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101612357A (en) * | 2009-02-13 | 2009-12-30 | 西安正大制药有限公司 | A kind of Chinese medicine composition for the treatment of tumor and preparation method thereof |
| CN101987124A (en) * | 2009-08-06 | 2011-03-23 | 江西省中医药研究院 | Traditional Chinese medicine composition for treating dyspepsia and preparation method thereof |
| CN102048941A (en) * | 2009-11-03 | 2011-05-11 | 天津中新药业集团股份有限公司达仁堂制药厂 | Quality control method of children-welfare tablets serving as Chinese medicinal preparation |
-
2012
- 2012-07-12 CN CN201210241372.4A patent/CN103543214B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101612357A (en) * | 2009-02-13 | 2009-12-30 | 西安正大制药有限公司 | A kind of Chinese medicine composition for the treatment of tumor and preparation method thereof |
| CN101987124A (en) * | 2009-08-06 | 2011-03-23 | 江西省中医药研究院 | Traditional Chinese medicine composition for treating dyspepsia and preparation method thereof |
| CN102048941A (en) * | 2009-11-03 | 2011-05-11 | 天津中新药业集团股份有限公司达仁堂制药厂 | Quality control method of children-welfare tablets serving as Chinese medicinal preparation |
Non-Patent Citations (3)
| Title |
|---|
| 文才华 等: "高效液相色谱法测定平消片中柚皮苷的含量", 《临床合理用药》 * |
| 杨武亮 等: "高效液相色谱法测定不同产地枳壳中柚皮苷和新橙皮苷", 《中草药》 * |
| 王发英 等: "枳壳质量标准研究", 《中成药》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110988159A (en) * | 2019-11-25 | 2020-04-10 | 通化卫京药业股份有限公司 | Method for measuring contents of multiple components of Jingyaokang capsule |
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