CN101320026A - Quality detection method of novel healing formulation - Google Patents
Quality detection method of novel healing formulation Download PDFInfo
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- CN101320026A CN101320026A CNA2008101167726A CN200810116772A CN101320026A CN 101320026 A CN101320026 A CN 101320026A CN A2008101167726 A CNA2008101167726 A CN A2008101167726A CN 200810116772 A CN200810116772 A CN 200810116772A CN 101320026 A CN101320026 A CN 101320026A
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Abstract
The invention relates to a quality detection method of a rehabilitation new preparation which is made from barbaric cockroach (American cockroach) drug material and the extract thereof. The quality detection method of the rehabilitation new preparation is constructed through a plurality of experiments. In said method, octadecylsilane chemically bonded silica is used as filling agent; diammonium phosphate is used as mobile phase; uracil is added with to be dissolved as reference solution; high performance liquid chromatography is used for detecting the sample solution of the rehabilitation new preparation to obtain the content determining method of the uracil in the rehabilitation new preparation. The method is relatively simple, is provided good precision, reproducibility and reliability and can be applied to the quality control of the rehabilitation new preparation.
Description
Technical field
The present invention relates to a kind of quality determining method, particularly a kind of quality determining method of kangfuxin.
Background technology
The new liquid of rehabilitation records in the 19 of Drug Standard of Ministry of Public Health of the Peoples Republic of China (Chinese patent drug) and WS3-B-3674-2000 (Z) " the new liquid of rehabilitation ", is the preparation of being made by American-cockroach-extract, have promoting blood circulation, the effect of nourishing yin and promoting granulation.Be used for stagnation of blood stasis, it is hemorrhage to have a stomachache, stomach, duodenal ulcer; And deficiency of Yin tuberculosis, phthisical supplemental treatment has good result.Because of its good effect, instant effect, and be widely used in clinical.
Principal ingredient is amino acid (alanine, leucine, isoleucine etc.) and alkaloid (uracil etc.) in the new liquid of rehabilitation.Only carried out the discriminating of assay, amino acid and the uracil of total amino acid in the new liquid quality standard of rehabilitation, above method all can not be controlled the new liquid quality of rehabilitation preferably, the particularly main alkaloidal quality control of effective constituent.Measure and still do not have report so far and rough Lian (American cockroach) medicinal material and extract are made in the kangfuxin alkaloidal HPLC method, and directly extract, filtering the preparation need testing solution measures, the result is because after having a large amount of various auxiliary material dissolvings in the kangfuxin, cause poor reproducibility, chromatographic column is imitated problems such as serious reduction carrying out about 10 pin left and right sides posts.
Summary of the invention
One object of the present invention is to disclose a kind of quality determining method of kangfuxin.
The present invention seeks to be achieved through the following technical solutions:
The content assaying method of the new solid pharmaceutical preparation of rehabilitation of the present invention, this method comprises the steps:
A. the preparation of need testing solution: rehabilitation new tablets porphyrize or capsule inclined content, accurate fixed solid preparation powder or particle 0.2～10 weight portion of claiming, put in the 25 parts by volume measuring bottles, add water 5～20 parts by volume, sonicated 10～60 minutes, thin up shakes up to scale, filter, get subsequent filtrate; Get Zeo-karb, grind, cross 50 mesh sieves and remove coarse grain, remove particulate after 150 mesh sieves, be soaked in water 16～32 hours, soaked 1～3 hour with the 2mol/L hydrochloric acid solution of 2～3 times of amounts the incline back of anhydrating, and stir 2～6 times at the interval, removes acid solution, wash with water to nearly neutrality, the 1mol/L sodium hydroxide solution that adds 2～6 times of amounts soaked 1～3 hour, stirred 2～6 times at interval, removed alkali lye, wash with water to nearly neutrality, the 2mol/L hydrochloric acid solution that adds 2～4 times of amounts soaked 1～3 hour, stirred 2～6 times at interval, remove acid solution, wash with water to nearly neutrality, soak in the water and place, standby; Precision is measured subsequent filtrate 8～12 parts by volume, is added on the cation exchange resin column of having handled well, collects effluent, with 5～10 parts by volume water washing cation exchange resin columns, collect cleansing solution, merge, be transferred in the 25 parts by volume measuring bottles with effluent, add water to scale, shake up, standby;
B. the preparation of reference substance solution: take by weighing uracil, add water and make the solution that every parts by volume contains uracil 0.0002～0.1 weight portion, in contrast product solution;
C. measure: the chromatographic column filling agent is an octadecylsilane chemically bonded silica; Ammonium dibasic phosphate solution with 0.01～0.2mol/L is a moving phase; The detection wavelength is 250～270nm; Accurate need testing solution and each 0.005～0.05 parts by volume injection liquid chromatograph of reference substance solution drawn according to high effective liquid chromatography for measuring, calculates, promptly; The new solid pharmaceutical preparation of rehabilitation of the present invention per diem taking dose meter contains uracil, must not be lower than 0.0001 weight portion.
The uracil content assaying method of rehabilitation new liq preparation of the present invention, this method comprises the steps:
A. the preparation of need testing solution: get Zeo-karb, grind, cross 50 mesh sieves and remove coarse grain, remove particulate after 150 mesh sieves, be soaked in water 16～32 hours, soaked 1～3 hour with the 2mol/L hydrochloric acid solution of 2～3 times of amounts the incline back of anhydrating, and stir 2～6 times at the interval, removes acid solution, wash with water to nearly neutrality, the 1mol/L sodium hydroxide solution that adds 2～6 times of amounts soaked 1～3 hour, stirred 2～6 times at interval, removed alkali lye, wash with water to nearly neutrality, the 2mol/L hydrochloric acid solution that adds 2～4 times of amounts soaked 1～3 hour, stirred 2～6 times at interval, remove acid solution, wash with water to nearly neutrality, soak in the water and place, standby; Accurate rehabilitation new liq preparation 5～20 parts by volume of drawing are added on the cation exchange resin column of having handled well, collect effluent, with 5～20 parts by volume water washing cation exchange resin columns, collect cleansing solution, merge, concentrate with effluent, be transferred in the 8-12 parts by volume measuring bottle, add water to scale, shake up, standby;
B. the preparation of reference substance solution: take by weighing uracil, add water and make the solution that every parts by volume contains uracil 0.0002～0.1 weight portion, in contrast product solution;
C. measure: the chromatographic column filling agent is an octadecylsilane chemically bonded silica; Ammonium dibasic phosphate solution with 0.01～0.2mol/L is a moving phase; The detection wavelength is 250～270nm; Accurate need testing solution and each 0.005～0.05 parts by volume injection liquid chromatograph of reference substance solution drawn according to high effective liquid chromatography for measuring, calculates, promptly; Rehabilitation new liq preparation of the present invention per diem taking dose meter contains uracil, must not be lower than 0.0001 weight portion.
The uracil content assaying method of the new solid pharmaceutical preparation of rehabilitation of the present invention, this method is preferably as follows step:
A. the preparation of need testing solution: rehabilitation new tablets porphyrize or capsule inclined content, and accurate fixed solid preparation powder or particle 1.0 weight portions of claiming are put in the 25 parts by volume measuring bottles, add water 20 parts by volume, sonicated 30 minutes, thin up is to scale, shake up, filter, get subsequent filtrate; Get Zeo-karb, grind, cross 50 mesh sieves and remove coarse grain, remove particulate after 150 mesh sieves, be soaked in water 24 hours, soaked 2 hours with the 2mol/L hydrochloric acid solution of 2～3 times of amounts the incline back of anhydrating, and stir 4 times at the interval, removes acid solution, wash with water to nearly neutrality, the 1mol/L sodium hydroxide solution that adds 4 times of amounts soaked 2 hours, stirred 4 times at interval, removed alkali lye, wash with water to nearly neutrality, the 2mol/L hydrochloric acid solution that adds 3 times of amounts soaked 2 hours, stirred 4 times at interval, remove acid solution, wash with water to nearly neutrality, soak in the water and place, standby; Precision is measured subsequent filtrate 10 parts by volume and is added on the cation exchange resin column of having handled well, collects effluent, with 10 parts by volume water washing cation exchange resin columns, collect cleansing solution, merge, be transferred in the 25 parts by volume measuring bottles with effluent, add water to scale, shake up, standby;
B. the preparation of reference substance solution: take by weighing uracil, add water and make the solution that every parts by volume contains uracil 0.01 weight portion, in contrast product solution;
C. measuring the chromatographic column filling agent is octadecylsilane chemically bonded silica; Ammonium dibasic phosphate solution with 0.05mol/L is a moving phase; The detection wavelength is 259nm; Accurate need testing solution and each 0.02 parts by volume injection liquid chromatograph of reference substance solution drawn according to high effective liquid chromatography for measuring, calculates, promptly; The new solid pharmaceutical preparation of rehabilitation of the present invention per diem taking dose meter contains uracil, must not be lower than 0.0001 weight portion.
The uracil content assaying method of rehabilitation new liq preparation of the present invention, this method is preferably as follows step:
A. the preparation of need testing solution: get Zeo-karb, grind, cross 50 mesh sieves and remove coarse grain, remove particulate after 150 mesh sieves, be soaked in water 24 hours, soaked 2 hours with the 2mol/L hydrochloric acid solution of 2～3 times of amounts the incline back of anhydrating, and stir 4 times at the interval, removes acid solution, wash with water to nearly neutrality, the 1mol/L sodium hydroxide solution that adds 4 times of amounts soaked 2 hours, stirred 4 times at interval, removed alkali lye, wash with water to nearly neutrality, the 2mol/L hydrochloric acid solution that adds 3 times of amounts soaked 2 hours, stirred 4 times at interval, remove acid solution, wash with water to nearly neutrality, soak in the water and place, standby; Accurate rehabilitation new liq preparation 10 parts by volume of drawing are added on the cation exchange resin column of having handled well, collect effluent, with 10 parts by volume water washing cation exchange resin columns, collect cleansing solution, merge with effluent, concentrate, be transferred in the 10 parts by volume measuring bottles, add water to scale, shake up, standby;
B. the preparation of reference substance solution: take by weighing uracil, add water and make the solution that every parts by volume contains uracil 0.01 weight portion, in contrast product solution;
C. measure: the chromatographic column filling agent is an octadecylsilane chemically bonded silica; Ammonium dibasic phosphate solution with 0.05mol/L is a moving phase; The detection wavelength is 259nm; Accurate need testing solution and each 0.02 parts by volume injection liquid chromatograph of reference substance solution drawn according to high effective liquid chromatography for measuring, calculates, promptly; Rehabilitation new liq preparation of the present invention per diem taking dose meter contains uracil, must not be lower than 0.0001 weight portion.
Wherein, kangfuxin of the present invention is by (Chinese patent drug) the 19 and WS3-B-3674-2000 (Z) " the new liquid of rehabilitation ", adds tablet, capsule, powder, soft capsule, dripping pill, honeyed bolus, pill, granule, soft extract with bee honey agent, sustained release preparation, quick releasing formulation, controlled release preparation, oral liquid or the ejection preparation that conventional auxiliary material is made according to conventional method.
The ratio of weight portion of the present invention and parts by volume is a grams per milliliter.Kangfuxin quality determining method of the present invention can be applied to the various formulations of composition, as tablet, capsule, oral liquid, dripping pill, spray, clinical acceptable forms such as granule, because in the wherein contained suitable American-cockroach-extract amount of the preparation of amino acid different dosage form is identical, therefore each formulation is when carrying out quality control, selected sample size can unify to convert the suitable American-cockroach-extract amount in amino acid, this quality determining method is in amino acid, with suitable American-cockroach-extract amount 3.0-16.0mg is the per unit preparation, and the per unit preparation can be for every, every, every (10ml/ props up) or every ball etc.
The inventive method is as follows with the progressive that existing kangfuxin quality determining method is compared: this method has overcome the defective that the national standard detection method does not have uracil assay index, solved since wherein adjunct ingredient cause poor reproducibility and chromatographic column post to imitate the problem that reduces, realized assay to uracil in the kangfuxin.Uracil content assaying method of the present invention has effectively been controlled the content of uracil in the kangfuxin; Uracil content assaying method of the present invention can effectively be controlled the quality of being made by rough Lian (American cockroach) extract including but not limited to preparations such as the new liquid of rehabilitation, rehabilitation new capsule, rehabilitation new film and the new sprays of rehabilitation; Uracil content assaying method provided by the invention can be used as the key means of estimating the kangfuxin traditional Chinese medicine quality, helps the modernization of Chinese medicine.
Description of drawings:
Fig. 1: uracil linear relationship
Following experimental example and embodiment are used for further specifying but are not limited to the present invention.
Experimental example 1 improves post effect and reproducible test results
1, instrument and reagent
Waters2695-2996 PDAD-Empower work station.
Kangfuxin: Kangfuxin Liquid: Hunan Central South Kelun Medicine Co., Ltd.'s (lot number: 061202); Rehabilitation new capsule: Sichuan Pearl Pharmaceutical Co., Ltd's (lot number: 051001).
Uracil reference substance: check institute, lot number: 100469-200401 available from Chinese pharmaceutical biological product.
2, chromatographic condition
C-18 chromatographic column (Alltima C18, 250mm * 4.6mm, 5 μ m); Mobile phase is: 0.05mol/L Ammonium dibasic phosphate solution; Column temperature: 35 ℃; Detect wavelength: 259nm.
3, test method and result
3.1 the preparation of need testing solution:
3.1.1 get rehabilitation new capsule content 0.4g, accurately weighed, put in the 25ml measuring bottle, add water 20ml, Ultrasonic processing (power 250W, frequency 50kHz) 30 minutes, thin up shakes up to scale, filters, Namely get need testing solution.
3.1.2 get Kangfuxin Liquid 10ml, filter, namely get need testing solution.
3.2 the preparation of reference substance solution: precision takes by weighing uracil reference substance 5.12mg, adds water and makes every 1ml Contain the uracil reference substance storing solution of uracil 0.1024mg, precision is measured uracil reference substance storing solution 1ml puts in the 10ml measuring bottle, is diluted with water to scale, shakes up, and namely gets every 1ml and contains uracil 10.24 The uracil reference substance solution of μ g.
3.3 continuous sample introduction post effect is analyzed: precision is drawn need testing solution 20 μ l, continuous sample introduction 6 respectively Pin calculates separating degree and post effect. The results are shown in Table 1.
Table 1 kangfuxin continuous sample introduction post effect is analyzed
Annotate: method 1 is cation seperation column need testing solution preparation method only; Method 2 supplies for cation seperation column The test sample solution preparation method.
As seen from Table 1, employing method 2 theoretical cam curves and separating degree are stable, and the chromatographic column post is imitated not with advancing The increase of going changes, and employing method 1 theoretical cam curve and separating degree all reduce gradually, the post effect Descend.
3.4 reproducible impact: 6 parts of each sample samplings prepare test sample according to experimental example 1 method Solution is also analyzed, and the result adopts and carries out reappearance experiment, the RSD% branch of rehabilitation new capsule and Kangfuxin Liquid Be not: 4.27%, 4.40%. The reappearance of illustration method 1 is undesirable, the reappearance ideal of method 2.
The quality testing experiment of experimental example 2 kangfuxins
1, instrument and reagent
Waters2695-2996 PDAD-Empower work station.
Kangfuxin: the new liquid of rehabilitation: Hunan Central South Kelun Medicine Co., Ltd.'s (lot number: 061202,061226,061228); The new spray of rehabilitation: Hunan Central South Kelun Medicine Co., Ltd.'s (lot number: 051001,051002,051003); Rehabilitation new capsule: Sichuan Pearl Pharmaceutical Co., Ltd's (lot number: 051001,051002,051003); Rehabilitation new film: Sichuan Pearl Pharmaceutical Co., Ltd's (lot number: 051001,051002,051003); The new soft capsule of rehabilitation: Sichuan Pearl Pharmaceutical Co., Ltd's (lot number: 051001,051002,051003); The new particle of rehabilitation: Sichuan Pearl Pharmaceutical Co., Ltd's (lot number: 051001,051002,051003).
Uracil reference substance: check institute, lot number: 100469-200401 available from Chinese pharmaceutical biological product.
2, maximum absorption wavelength is determined
Adopt PDA that uracil is carried out the mensuration of maximum absorption band, test findings shows that uracil is in 250～270nm scope, and peak area changes less, and the place has absorption maximum at the 259nm wavelength.
3, chromatographic condition
C-18 chromatographic column (Alltima C
18, 250mm * 4.6mm, 5 μ m; Alltima C
18, 150mm * 3.9mm, 5 μ m; Inertsil ODS3,250mm * 4.6mm, 5 μ m; Phenomenex C
18, 250mm * 4.6mm, 5 μ m); Moving phase is: the ammonium dibasic phosphate solution of 0.05mol/L; Column temperature: 35 ℃; Detect wavelength: 259nm.
4, test method and result
4.1 the preparation of need testing solution:
4.1.1 get rehabilitation new capsule content 1g, the accurate title, decide, and puts in the 25ml measuring bottle, adds water 20ml, sonicated (power 250W, frequency 50kHz) 30 minutes, and thin up shakes up to scale, filters.Precision is measured subsequent filtrate 10ml, is added on the cation exchange resin column of having handled well, collects effluent, uses the 10ml water washing, collects cleansing solution, merges with effluent, puts in the 25ml measuring bottle, adds water to scale, shakes up, and promptly gets need testing solution.
4.1.2 get 20 of rehabilitation new films, porphyrize is got about 1g, the accurate title, decide, and puts in the 25ml measuring bottle, adds water 20ml, sonicated (power 250W, frequency 50kHz) 30 minutes, and thin up shakes up to scale, filters.Precision is measured subsequent filtrate 10ml, is added on the cation exchange resin column of having handled well, collects effluent, uses the 10ml water washing, collects cleansing solution, merges with effluent, puts in the 25ml measuring bottle, adds water to scale, shakes up, and promptly gets need testing solution.
4.1.3 get the about 10g of the new particle of rehabilitation, the accurate title, decide, and puts in the 25ml measuring bottle, adds water 20ml, sonicated (power 250W, frequency 50kHz) 30 minutes, and thin up shakes up to scale, filters.Precision is measured subsequent filtrate 10ml, is added on the cation exchange resin column of having handled well, collects effluent, uses the 10ml water washing, collects cleansing solution, merges with effluent, puts in the 25ml measuring bottle, adds water to scale, shakes up, and promptly gets need testing solution.
4.1.4 get the new liquid of rehabilitation/spray 10ml, be added on the cation exchange resin column of having handled well, collect effluent, use the 10ml water washing, collect cleansing solution, merge, be concentrated in right amount, put in the 10ml measuring bottle with effluent, add water to scale, shake up, promptly get need testing solution.
4.1.5 get the about 2g of the new soft capsule content of rehabilitation, be added on the cation exchange resin column of having handled well, collect effluent, use the 20ml water washing, collect cleansing solution, merge, be concentrated in right amount, put in the 10ml measuring bottle with effluent, add water to scale, shake up, promptly get need testing solution.
4.2 the preparation of reference substance solution: precision takes by weighing uracil reference substance 5.12mg, add water and make the uracil reference substance storing solution that every 1ml contains uracil 0.1024mg, precision is measured uracil reference substance storing solution lml, put in the 10ml measuring bottle, be diluted with water to scale, shake up, promptly get the uracil reference substance solution that every 1ml contains uracil 10.24 μ g.
4.3 content assaying method: accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly.The results are shown in Table 2.
Table 2 kangfuxin assay result
Annotate: solid pharmaceutical preparation unit is: μ g/ grain, μ g/g, μ g/ sheet; Liquid preparation unit is: μ g/ml
Experimental example 3 kangfuxin content assaying method experiments of the present invention
1, quantitative limit and detectability: the uracil reference substance solution of the accurate 10.24 μ g/ml of absorption is injected liquid chromatograph, the record chromatogram, when observation signal is 10 times of noise levels, sampling volume is 0.5 μ l, and sample size is 5.12ng, promptly quantitatively is limited to 5.12ng, when observation signal is 3 times of noise levels, sampling volume is 0.2 μ l, and sample size is 2.048ng, promptly detects and is limited to 2.048ng;
2, the investigation of linear relationship: the uracil reference substance solution 0.5 μ l of the accurate 10.24 μ g/ml of absorption and accurate uracil reference substance solution 0.1 μ l, 0.2 μ l, 0.5 μ, 1,1 μ l, 2 μ l, 5 μ l, 10 μ l, the 20 μ l that draw 0.1024mg/ml, inject high performance liquid chromatograph, ammonium dibasic phosphate solution with 0.05mol/L is a moving phase, measure peak area with aforementioned chromatographic condition, determination data sees Table 15-16, (μ g) is ordinate with the uracil sample size, peak area is a horizontal ordinate, the drawing standard curve is as follows, the results are shown in Table 3:
Table 3 linear relationship is investigated
※: uracil reference substance solution concentration: 0.1024mg/ml and 10.24 μ g/ml
Calculate regression equation: Y (μ g)=2.40407 * 10
-7X-0.00463
r＝0.99998
Linear relationship is investigated the result and proved: uracil sample introduction in 0.00512～2.048 μ g scope has good linear relationship; See Fig. 1.
3, precision test: the accurate uracil reference substance solution of drawing, repeat sample introduction 6 times, each 2 μ l carry out the precision test, the results are shown in Table 4;
Table 4 Precision test result
Above test findings proves: this method has good precision;
4, reappearance test: get the new liquid of rehabilitation (lot number 061202), rehabilitation new film (lot number 051001), rehabilitation new capsule (lot number 051001), the new spray of rehabilitation (lot number 051001), the new particle of rehabilitation (lot number 051001), the new soft capsule of rehabilitation (lot number 051001), 6 parts of each sample samplings, prepare need testing solution and analysis according to experimental example 1 method, 6 reproducible RSD% of formulation are respectively as a result: 1.03%, 1.40%, 0.38%, 1.15%, 0.92%, 1.27%;
5, stability test: get reappearance test item each portion of need testing solution down, measure respectively at 0,3.5,24 hour, the RSD% of new 6 the preparation chromatographic peak peak areas of rehabilitation is respectively: 0.63%, 0.18%, 1.50%, 0.79%, 1.21%, 1.09%;
6, the application of sample recovery test: precision takes by weighing/draws the new liquid of rehabilitation (5ml) of known content, rehabilitation new film (0.5g), rehabilitation new capsule (0.5g), the new spray of rehabilitation (5ml), the new particle of rehabilitation (5g), the new soft capsule of rehabilitation (1g), add uracil reference substance 51.2 μ g respectively, 0.3072mg, 0.3072mg, 51.2 μ g, 0.3072mg, 0.3072mg, 6 parts of each sample samplings, prepare need testing solution and analysis according to experimental example 1 method, 6 formulation average recoveries are respectively as a result: 1.37%, 0.38%, 1.18%, 1.47%, 0.98%, 1.32%;
Following embodiment all can realize the effect of above-mentioned experimental example.
Embodiment
Embodiment 1: the uracil content assaying method of rehabilitation virgin rubber wafer of the present invention, this method comprises the steps:
A. the preparation of need testing solution: rehabilitation virgin rubber wafer inclined content, and accurate the title decide content 1.0g, puts in the 25ml measuring bottle, adds water 20ml, sonicated 30 minutes, and thin up shakes up to scale, filters, must subsequent filtrate; Get Zeo-karb, grind, cross 50 mesh sieves and remove coarse grain, remove particulate after 150 mesh sieves, be soaked in water 24 hours, soaked 2 hours with the 2mol/L hydrochloric acid solution of 2～3 times of amounts the incline back of anhydrating, and stir 4 times at the interval, removes acid solution, wash with water to nearly neutrality, the 1mol/L sodium hydroxide solution that adds 4 times of amounts soaked 2 hours, stirred 4 times at interval, removed alkali lye, wash with water to nearly neutrality, the 2mol/L hydrochloric acid solution that adds 3 times of amounts soaked 2 hours, stirred 4 times at interval, remove acid solution, wash with water to nearly neutrality, soak in the water and place, standby; Precision is measured subsequent filtrate 10ml, is added on the cation exchange resin column of having handled well, collects effluent, with 10ml water washing cation exchange resin column, collects cleansing solution, merges with effluent, is transferred in the 25ml measuring bottle, adds water to scale, shakes up, and is standby;
B. the preparation of reference substance solution: take by weighing uracil, add water and make the solution that every 1ml contains uracil 0.01g, in contrast product solution;
C. measuring the chromatographic column filling agent is octadecylsilane chemically bonded silica; Ammonium dibasic phosphate solution with 0.05mol/L is a moving phase; The detection wavelength is 259nm; Accurate need testing solution and each 0.02ml injection liquid chromatograph of reference substance solution drawn according to high effective liquid chromatography for measuring, calculates, promptly; Rehabilitation new capsule of the present invention contains uracil, and every must not be lower than 60.0 μ g.
Embodiment 2: the uracil content assaying method of rehabilitation new tablets of the present invention, this method comprises the steps:
A. the preparation of need testing solution: with rehabilitation new tablets porphyrize, the accurate title, decided powder 1.0g, puts in the 25ml measuring bottle, adds water 20ml, sonicated 30 minutes, and thin up shakes up to scale, filters, and gets subsequent filtrate; Get Zeo-karb, grind, cross 50 mesh sieves and remove coarse grain, remove particulate after 150 mesh sieves, be soaked in water 24 hours, soaked 2 hours with the 2mol/L hydrochloric acid solution of 2～3 times of amounts the incline back of anhydrating, and stir 4 times at the interval, removes acid solution, wash with water to nearly neutrality, the 1mol/L sodium hydroxide solution that adds 4 times of amounts soaked 2 hours, stirred 4 times at interval, removed alkali lye, wash with water to nearly neutrality, the 2mol/L hydrochloric acid solution that adds 3 times of amounts soaked 2 hours, stirred 4 times at interval, remove acid solution, wash with water to nearly neutrality, soak in the water and place, standby; Precision is measured subsequent filtrate 10ml, is added on the cation exchange resin column of having handled well, collects effluent, with 10ml water washing cation exchange resin column, collects cleansing solution, merges with effluent, is transferred in the 25ml measuring bottle, adds water to scale, shakes up, and is standby;
B. the preparation of reference substance solution: take by weighing uracil, add water and make the solution that every 1ml contains uracil 0.01g, in contrast product solution;
C. measuring the chromatographic column filling agent is octadecylsilane chemically bonded silica; Ammonium dibasic phosphate solution with 0.05mol/L is a moving phase; The detection wavelength is 259nm; Accurate need testing solution and each 0.02ml injection liquid chromatograph of reference substance solution drawn according to high effective liquid chromatography for measuring, calculates, promptly; Rehabilitation new film of the present invention contains uracil, and every must not be lower than 60.0 μ g.
Embodiment 3: the uracil content assaying method of the new liquid of rehabilitation of the present invention, this method comprises the steps:
A. the preparation of need testing solution: get Zeo-karb, grind, cross 50 mesh sieves and remove coarse grain, remove particulate after 150 mesh sieves, be soaked in water 24 hours, soaked 2 hours with the 2mol/L hydrochloric acid solution of 2～3 times of amounts the incline back of anhydrating, and stir 4 times at the interval, removes acid solution, wash with water to nearly neutrality, the 1mol/L sodium hydroxide solution that adds 4 times of amounts soaked 2 hours, stirred 4 times at interval, removed alkali lye, wash with water to nearly neutrality, the 2mol/L hydrochloric acid solution that adds 3 times of amounts soaked 2 hours, stirred 4 times at interval, remove acid solution, wash with water to nearly neutrality, soak in the water and place, standby; The accurate rehabilitation new liq preparation 10ml that draws is added on the cation exchange resin column of having handled well, collects effluent, with 10ml water washing cation exchange resin column, collect cleansing solution, merge, concentrate, be transferred in the 10ml measuring bottle with effluent, add water to scale, shake up, standby;
B. the preparation of reference substance solution: take by weighing uracil, add water and make the solution that every 1ml contains uracil 0.01g, in contrast product solution;
C. measure: the chromatographic column filling agent is an octadecylsilane chemically bonded silica; Ammonium dibasic phosphate solution with 0.05mol/L is a moving phase; The detection wavelength is 259nm; Accurate need testing solution and each 0.02 parts by volume injection liquid chromatograph of reference substance solution drawn according to high effective liquid chromatography for measuring, calculates, promptly; The new liquid of rehabilitation of the present invention contains uracil, and every 1ml must not be lower than 6.0 μ g.
Embodiment 4: the uracil content assaying method of the new spray of rehabilitation of the present invention, this method comprises the steps:
A. the preparation of need testing solution: get Zeo-karb, grind, cross 50 mesh sieves and remove coarse grain, remove particulate after 150 mesh sieves, be soaked in water 24 hours, soaked 2 hours with the 2mol/L hydrochloric acid solution of 2～3 times of amounts the incline back of anhydrating, and stir 4 times at the interval, removes acid solution, wash with water to nearly neutrality, the 1mol/L sodium hydroxide solution that adds 4 times of amounts soaked 2 hours, stirred 4 times at interval, removed alkali lye, wash with water to nearly neutrality, the 2mol/L hydrochloric acid solution that adds 3 times of amounts soaked 2 hours, stirred 4 times at interval, remove acid solution, wash with water to nearly neutrality, soak in the water and place, standby; The accurate rehabilitation new liq preparation 10ml that draws is added on the cation exchange resin column of having handled well, collects effluent, with 10ml water washing cation exchange resin column, collect cleansing solution, merge, concentrate, be transferred in the 10ml measuring bottle with effluent, add water to scale, shake up, standby;
B. the preparation of reference substance solution: take by weighing uracil, add water and make the solution that every 1ml contains uracil 0.01g, in contrast product solution;
C. measure: the chromatographic column filling agent is an octadecylsilane chemically bonded silica; Ammonium dibasic phosphate solution with 0.05mol/L is a moving phase; The detection wavelength is 259nm; Accurate need testing solution and each 0.02 parts by volume injection liquid chromatograph of reference substance solution drawn according to high effective liquid chromatography for measuring, calculates, promptly; The new spray of rehabilitation of the present invention contains uracil, must not be lower than 6.0 μ g.
Embodiment 5: the uracil content assaying method of the new soft capsule of rehabilitation of the present invention, this method comprises the steps:
A. the preparation of need testing solution: rehabilitation virgin rubber wafer inclined content, and accurate the title decide content 2.0g, puts in the 25ml measuring bottle, adds water 20ml, sonicated 30 minutes, and thin up shakes up to scale, filters, must subsequent filtrate; Get Zeo-karb, grind, cross 50 mesh sieves and remove coarse grain, remove particulate after 150 mesh sieves, be soaked in water 24 hours, soaked 2 hours with the 2mol/L hydrochloric acid solution of 2～3 times of amounts the incline back of anhydrating, and stir 4 times at the interval, removes acid solution, wash with water to nearly neutrality, the 1mol/L sodium hydroxide solution that adds 4 times of amounts soaked 2 hours, stirred 4 times at interval, removed alkali lye, wash with water to nearly neutrality, the 2mol/L hydrochloric acid solution that adds 3 times of amounts soaked 2 hours, stirred 4 times at interval, remove acid solution, wash with water to nearly neutrality, soak in the water and place, standby; Precision is measured subsequent filtrate 10ml, is added on the cation exchange resin column of having handled well, collects effluent, with 10ml water washing cation exchange resin column, collects cleansing solution, merges with effluent, is transferred in the 10ml measuring bottle, adds water to scale, shakes up, and is standby;
B. the preparation of reference substance solution: take by weighing uracil, add water and make the solution that every 1ml contains uracil 0.01g, in contrast product solution;
C. measuring the chromatographic column filling agent is octadecylsilane chemically bonded silica; Ammonium dibasic phosphate solution with 0.05mol/L is a moving phase; The detection wavelength is 259nm; Accurate need testing solution and each 0.02ml injection liquid chromatograph of reference substance solution drawn according to high effective liquid chromatography for measuring, calculates, promptly; The new soft capsule of rehabilitation of the present invention contains uracil, and every must not be lower than 60.0 μ g.
Embodiment 6: the uracil content assaying method of the new granule of rehabilitation of the present invention, this method comprises the steps:
A. the preparation of need testing solution: get the new granule of rehabilitation, the accurate title, decided particle 10.0g, puts in the 25ml measuring bottle, adds water 20ml, sonicated 30 minutes, and thin up shakes up to scale, filters, and gets subsequent filtrate; Get Zeo-karb, grind, cross 50 mesh sieves and remove coarse grain, remove particulate after 150 mesh sieves, be soaked in water 24 hours, soaked 2 hours with the 2mol/L hydrochloric acid solution of 2～3 times of amounts the incline back of anhydrating, and stir 4 times at the interval, removes acid solution, wash with water to nearly neutrality, the 1mol/L sodium hydroxide solution that adds 4 times of amounts soaked 2 hours, stirred 4 times at interval, removed alkali lye, wash with water to nearly neutrality, the 2mol/L hydrochloric acid solution that adds 3 times of amounts soaked 2 hours, stirred 4 times at interval, remove acid solution, wash with water to nearly neutrality, soak in the water and place, standby; Precision is measured subsequent filtrate 10ml, is added on the cation exchange resin column of having handled well, collects effluent, with 10ml water washing cation exchange resin column, collects cleansing solution, merges with effluent, is transferred in the 25ml measuring bottle, adds water to scale, shakes up, and is standby;
B. the preparation of reference substance solution: take by weighing uracil, add water and make the solution that every 1ml contains uracil 0.01g, in contrast product solution;
C. measuring the chromatographic column filling agent is octadecylsilane chemically bonded silica; Ammonium dibasic phosphate solution with 0.05mol/L is a moving phase; The detection wavelength is 259nm; Accurate need testing solution and each 0.02ml injection liquid chromatograph of reference substance solution drawn according to high effective liquid chromatography for measuring, calculates, promptly; The new particle of rehabilitation of the present invention contains uracil, and every g must not be lower than 20.0 μ g.
Claims (3)
1, a kind of quality determining method of kangfuxin is characterized in that this method is a kind of in the following method:
The quality determining method of the new solid pharmaceutical preparation of rehabilitation:
A. the preparation of need testing solution: rehabilitation new tablets porphyrize or capsule inclined content, accurate fixed solid preparation powder or particle 0.2～10 weight portion of claiming, put in the 25 parts by volume measuring bottles, add water 5～20 parts by volume, sonicated 10～60 minutes, thin up shakes up to scale, filter, get subsequent filtrate; Get Zeo-karb, grind, cross 50 mesh sieves and remove coarse grain, remove particulate after 150 mesh sieves, be soaked in water 16～32 hours, soaked 1～3 hour with the 2mol/L hydrochloric acid solution of 2～3 times of amounts the incline back of anhydrating, and stir 2～6 times at the interval, removes acid solution, wash with water to nearly neutrality, the 1mol/L sodium hydroxide solution that adds 2～6 times of amounts soaked 1～3 hour, stirred 2～6 times at interval, removed alkali lye, wash with water to nearly neutrality, the 2mol/L hydrochloric acid solution that adds 2～4 times of amounts soaked 1～3 hour, stirred 2～6 times at interval, remove acid solution, wash with water to nearly neutrality, soak in the water and place, standby; Precision is measured subsequent filtrate 8～12 parts by volume, is added on the cation exchange resin column of having handled well, collects effluent, with 5～10 parts by volume water washing cation exchange resin columns, collect cleansing solution, merge, be transferred in the 25 parts by volume measuring bottles with effluent, add water to scale, shake up, standby;
B. the preparation of reference substance solution: take by weighing uracil, add water and make the solution that every parts by volume contains uracil 0.0002～0.1 weight portion, in contrast product solution;
C. measure: the chromatographic column filling agent is an octadecylsilane chemically bonded silica; Ammonium dibasic phosphate solution with 0.01～0.2mol/L is a moving phase; The detection wavelength is 250～270nm; Accurate need testing solution and each 0.005～0.05 parts by volume injection liquid chromatograph of reference substance solution drawn according to high effective liquid chromatography for measuring, calculates, promptly; The new solid pharmaceutical preparation of rehabilitation of the present invention per diem taking dose meter contains uracil, must not be lower than 0.0001 weight portion;
Or the quality determining method of rehabilitation new liq preparation:
A. the preparation of need testing solution: get Zeo-karb, grind, cross 50 mesh sieves and remove coarse grain, remove particulate after 150 mesh sieves, be soaked in water 16～32 hours, soaked 1～3 hour with the 2mol/L hydrochloric acid solution of 2～3 times of amounts the incline back of anhydrating, and stir 2～6 times at the interval, removes acid solution, wash with water to nearly neutrality, the 1mol/L sodium hydroxide solution that adds 2～6 times of amounts soaked 1～3 hour, stirred 2～6 times at interval, removed alkali lye, wash with water to nearly neutrality, the 2mol/L hydrochloric acid solution that adds 2～4 times of amounts soaked 1～3 hour, stirred 2～6 times at interval, remove acid solution, wash with water to nearly neutrality, soak in the water and place, standby; Accurate rehabilitation new liq preparation 5～20 parts by volume of drawing are added on the cation exchange resin column of having handled well, collect effluent, with 5～20 parts by volume water washing cation exchange resin columns, collect cleansing solution, merge, concentrate with effluent, be transferred in the 10 parts by volume measuring bottles, add water to scale, shake up, standby;
B. the preparation of reference substance solution: take by weighing uracil, add water and make the solution that every parts by volume contains uracil 0.0002～0.1 weight portion, in contrast product solution;
C. measure: the chromatographic column filling agent is an octadecylsilane chemically bonded silica; Ammonium dibasic phosphate solution with 0.01～0.2mol/L is a moving phase; The detection wavelength is 250～270nm; Accurate need testing solution and each 0.005～0.05 parts by volume injection liquid chromatograph of reference substance solution drawn according to high effective liquid chromatography for measuring, calculates, promptly; Rehabilitation new liq preparation of the present invention per diem taking dose meter contains uracil, must not be lower than 0.0001 weight portion.
2, quality determining method as claimed in claim 1 is characterized in that this method is a kind of in the following method:
The quality determining method of the new solid pharmaceutical preparation of rehabilitation:
A. the preparation of need testing solution: rehabilitation new tablets porphyrize or capsule inclined content, and accurate fixed solid preparation powder or particle 1.0 weight portions of claiming are put in the 25 parts by volume measuring bottles, add water 20 parts by volume, sonicated 30 minutes, thin up is to scale, shake up, filter, get subsequent filtrate; Get Zeo-karb, grind, cross 50 mesh sieves and remove coarse grain, remove particulate after 150 mesh sieves, be soaked in water 24 hours, soaked 2 hours with the 2mol/L hydrochloric acid solution of 2～3 times of amounts the incline back of anhydrating, and stir 4 times at the interval, removes acid solution, wash with water to nearly neutrality, the 1mol/L sodium hydroxide solution that adds 4 times of amounts soaked 2 hours, stirred 4 times at interval, removed alkali lye, wash with water to nearly neutrality, the 2mol/L hydrochloric acid solution that adds 3 times of amounts soaked 2 hours, stirred 4 times at interval, remove acid solution, wash with water to nearly neutrality, soak in the water and place, standby; Precision is measured subsequent filtrate 10 parts by volume and is added on the cation exchange resin column of having handled well, collects effluent, with 10 parts by volume water washing cation exchange resin columns, collect cleansing solution, merge, be transferred in the 25 parts by volume measuring bottles with effluent, add water to scale, shake up, standby;
B. the preparation of reference substance solution: take by weighing uracil, add water and make the solution that every parts by volume contains uracil 0.01 weight portion, in contrast product solution;
C. measuring the chromatographic column filling agent is octadecylsilane chemically bonded silica; Ammonium dibasic phosphate solution with 0.05mol/L is a moving phase; The detection wavelength is 259nm; Accurate need testing solution and each 0.02 parts by volume injection liquid chromatograph of reference substance solution drawn according to high effective liquid chromatography for measuring, calculates, promptly; The new solid pharmaceutical preparation of rehabilitation of the present invention per diem taking dose meter contains uracil, must not be lower than 0.0001 weight portion;
Or the quality determining method of rehabilitation new liq preparation:
A. the preparation of need testing solution: get Zeo-karb, grind, cross 50 mesh sieves and remove coarse grain, remove particulate after 150 mesh sieves, be soaked in water 24 hours, soaked 2 hours with the 2mol/L hydrochloric acid solution of 2～3 times of amounts the incline back of anhydrating, and stir 4 times at the interval, removes acid solution, wash with water to nearly neutrality, the 1mol/L sodium hydroxide solution that adds 4 times of amounts soaked 2 hours, stirred 4 times at interval, removed alkali lye, wash with water to nearly neutrality, the 2mol/L hydrochloric acid solution that adds 3 times of amounts soaked 2 hours, stirred 4 times at interval, remove acid solution, wash with water to nearly neutrality, soak in the water and place, standby; Accurate rehabilitation new liq preparation 10 parts by volume of drawing are added on the cation exchange resin column of having handled well, collect effluent, with 10 parts by volume water washing cation exchange resin columns, collect cleansing solution, merge with effluent, concentrate, be transferred in the 10 parts by volume measuring bottles, add water to scale, shake up, standby;
B. the preparation of reference substance solution: take by weighing uracil, add water and make the solution that every parts by volume contains uracil 0.01 weight portion, in contrast product solution;
C. measure: the chromatographic column filling agent is an octadecylsilane chemically bonded silica; Ammonium dibasic phosphate solution with 0.05mol/L is a moving phase; The detection wavelength is 259nm; Accurate need testing solution and each 0.02 parts by volume injection liquid chromatograph of reference substance solution drawn according to high effective liquid chromatography for measuring, calculates, promptly; Rehabilitation new liq preparation of the present invention per diem taking dose meter contains uracil, must not be lower than 0.0001 weight portion.
3, as claim 1,2 described quality determining methods, wherein the new solid pharmaceutical preparation of rehabilitation is selected from rehabilitation new capsule, rehabilitation new film, the new particle of rehabilitation, the new soft capsule of rehabilitation; Rehabilitation new liq preparation is selected from the new spray of rehabilitation, the new liquid of rehabilitation.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008101167726A CN101320026B (en) | 2008-07-17 | 2008-07-17 | Quality detection method of novel healing formulation |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103926350A (en) * | 2014-05-04 | 2014-07-16 | 昆明赛诺制药有限公司 | Inspection method of rehabilitation liquid formulation fingerprint and standard fingerprint |
| CN106370739A (en) * | 2016-08-18 | 2017-02-01 | 四川好医生攀西药业有限责任公司 | Kangfuxin solution preparation fingerprint quality determination method and standard fingerprint |
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2008
- 2008-07-17 CN CN2008101167726A patent/CN101320026B/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103926350A (en) * | 2014-05-04 | 2014-07-16 | 昆明赛诺制药有限公司 | Inspection method of rehabilitation liquid formulation fingerprint and standard fingerprint |
| CN106370739A (en) * | 2016-08-18 | 2017-02-01 | 四川好医生攀西药业有限责任公司 | Kangfuxin solution preparation fingerprint quality determination method and standard fingerprint |
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| CN101320026B (en) | 2011-09-07 |
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Assignee: Hunan Central South Kelun Medicine Co., Ltd. Assignor: Sichuan Kelun Pharmaceutical Co., Ltd. Contract record no.: 2011510000143 Denomination of invention: Quality detection method of novel healing formulation License type: Exclusive License Open date: 20081210 Record date: 20110812 |