CN101181590B - wei-xue-kang mastication tablet verification method - Google Patents
wei-xue-kang mastication tablet verification method Download PDFInfo
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Abstract
The invention relates to a quality standard and a testing method of the blood health chewable tablet. Through a plurality of tests, the Thin-Layer Chromatography identification and content determination items are set in the quality standard of the blood health chewable tablet, the quality testing method and standard of the blood health chewable tablet is provided, therefore the invention can effectively control the quality of the blood health chewable tablet, thus the quality of the blood health chewable tablet can be steady, controllable, efficient and safe; moreover, the invention can strictly control the feeding requirement and the quality of the product, overcome the defects of the prior art, and improve quality, curative effect and the bioavailability of the product. The product with high quality can ensure the curative effect, and preferably satisfy medical requirement. The invention improves the former quality standard, establishes the qualitative identification for the contained codonopsis pilosulas and fleece-flower roots, improves the qualitative identification for the contained dried old orange peel and establishes the content determination for the hesperidin which is contained in the dried old orange peel. Through the quality control of the invention, the quality of the blood health chewable tablet can be steady, controllable, efficient and safe.
Description
Technical field:
The present invention relates to a kind of quality standard and the method for inspection thereof of infantile health-care capsule chewable tablets.
Background technology:
Infantile health-care capsule chewable tablets side comes from " People's Republic of China's drug standards Chinese traditional patent formulation preparation " the 14 infantile health-care capsule syrup that records.Form by Radix Codonopsis, prepared rhizome of rehmannia, Chinese yam, dried orange peel, black soya bean, fructus amomi, the fleece-flower root, hawthorn, ferrous sulphate nine flavor medicines.The function kidney and spleen invigorating, the yin-nourishing of enriching blood.Be applicable to the spleen kidney deficiency, essence and blood loses empty, sallow complexion, and dizzy tinnitus, soreness and weakness of waist and knees, the burnout body is thin.Alimentary anemia or hypoferric anemia belong to above-mentioned patient.Be invigorating spleen and kidney, the good recipe of replenishing the vital essence and the blood.Former formulation is a syrup, and syrup has storage, transports, carries and take drawbacks such as inconvenience to a certain extent as liquid preparation.Because of primary standard only has the discriminating of medicinal material simply of proterties and dried orange peel, lack necessary medicine inherent quality prosecution index again, thereby limited the producing and selling and the clinical practice of this product to a certain extent.Therefore, we are on former side's technology basis, through Study on Forming, develop novel solid preparation---chewable tablets, and according to the technical requirement of relevant quality standard research in " the study of tcm new drug technical requirement " of National Drug Administration promulgation etc., adopt thin-layered chromatography, set up and worked out main thin layer identification system and the identification beacon of forming medicine in the infantile health-care capsule chewable tablets.Adopt the main contained main effective constituent Determination of Hesperidin Content of medicine dried orange peel of forming in the high effective liquid chromatography for measuring infantile health-care capsule chewable tablets.
Compare with former formulation, characteristics such as the infantile health-care capsule chewable tablets has storage, transports, carries, taking convenience and mouthfeel are good, have again quality controllable, safety and sanitation, novelty and feasibility such as medicine is stable.Thereby for exploitation infantile health-care capsule chewable tablets lays the foundation and foundation.
The infantile health-care capsule chewable tablets is the medicine of special for treating anaemia.We are the good recipe of clinical kidney and spleen invigorating, replenishing the vital essence and the blood.Utilization we's basic indication is: because the spleen kidney deficiency, essence and blood loses and causes sallow complexion, dizzy tinnitus, soreness and weakness of waist and knees, the category of the thin genus of burnout body motherland's medical science " deficiency of blood ".Modern medicine is referred to as " malnutritional anemia " and reaches " hypoferric anemia ".This disease belongs to common clinical, and frequently-occurring disease especially artificially to see in children, women, old age more.Take Radix Codonopsis, prepared rhizome of rehmannia tonifying middle-Jiao and Qi in the side, nourishing yin and supplementing blood is a monarch drug in a prescription, reuses Chinese yam, the dried orange peel eliminating dampness of regulating the flow of vital energy, and invigorating the spleen and stomach is a ministerial drug, assistant is with black soya bean, the fleece-flower root, hawthorn, fructus amomi etc., strengthening the spleen and stomach, and blood promotes the production of body fluid, all medicine compatibilities are played kidney and spleen invigorating altogether, and the good of the yin-nourishing of enriching blood imitated.
Radix Codonopsis: property is flat, and it is sweet to distinguish the flavor of, tool tonifying middle-Jiao and Qi, the effect of promoting the production of body fluid.For motherland's therapeutic treatment weakness of the spleen and the stomach, qi-blood deficiency, the key medicine of fatigue and asthenia etc." book on Chinese herbal medicine justice " carries: " Radix Codonopsis power energy tonifying spleen nourishing the stomach, moistening lung is promoted the production of body fluid, gas in the strong fortune, this is very mutually not far away with genseng.Its outstanding valuable person, invigorating the spleen fortune and not dry is then grown stomach-Yin and wet, and moistening lung and do not violate is cold and coolly nourished blood and is not grown greasyly partially, inspires middle-jiao yang, function of the spleen and stomach, gas in the vibration, and do not have dry fraud just ".Modern study proves: Radix Codonopsis has significant anti-hypoxia, anti-anaemia, effects such as antiulcer and enhancing body immunologic function.
Prepared rhizome of rehmannia: it is sweet, warm in nature to distinguish the flavor of, the function of tool nourishing yin and supplementing blood.It is few to control deficiency of Yin blood, waist knee flaccidity, deafness and blurred vision etc." detailed outline " said: " filling out marrow, promoting vital essence and blood genernation, tonifying five zang organs, promoting blood circulation, black beard and hair ... "." new compilation of materia medica " carries: " control all liver-kidney Yin deficiencies, deficient all kinds of diseases and ailments are the strengthening renal yin to inhibit predominant yang medicine ".Modern study proves: the many-sided significant physiologically active of prepared rhizome of rehmannia tool.Anti-ageing, enrich blood effects such as raise immunity.
Chinese yam: it is sweet to distinguish the flavor of, and property is flat, is invigorating the spleen, reinforces the kidney the product of benefit essence.It is few to cure mainly insufficiency of the spleen food, endless diarrhea, and emission due to the kidney deficiency, abnormal heat are quenched one's thirst etc.Modern pharmacological research proves: Chinese yam has the raising immunologic function, anti-anoxic, effect such as hypoglycemic grade.
Dried orange peel: bitter, suffering, temperature, the tool regulating qi-flowing for strengthening spleen, eliminating dampness and eliminating phlegm function is used for fullness and oppression of chest and abdomen, and the few vomiting and diarrhoea of food waits disease.Modern study proves: dried orange peel decocting liquid can make the saliva endo-amylase activity that exsomatizes increase, effects such as protection gastric mucosa, loose intestinal smooth muscle, anti-shock, anti-inflammatory antiallergy.
Summary of the invention
The object of the present invention is to provide a kind of quality standard and the method for inspection thereof of infantile health-care capsule chewable tablets,, can strengthen validity, quality controllability and the stability of this medicine by determining the quality standard and the method for inspection thereof.
The objective of the invention is to be achieved through the following technical solutions:
A kind of quality standard of infantile health-care capsule chewable tablets and the method for inspection thereof, its characteristics are: one or more that a discrimination method in this method and content assaying method are following method:
A differentiates:
The qualitative identification of Radix Codonopsis comprises the following steps: to get 10～20 of infantile health-care capsule chewable tablets, grinds, and adds ethanol 25～75ml, sonicated or hot reflux 15～45 minutes filter, and filtrate volatilizes, residue adds water 15～45ml makes dissolving, adds hydrochloric acid 1～3ml, methenyl choloride 15～45ml, reflux 20～60 minutes, put coldly, divide and to get methenyl choloride liquid, evaporate to dryness, residue adds methyl alcohol 0.5～1.5ml makes dissolving, as need testing solution.Other gets Radix Codonopsis control medicinal material 0.5～1.5g, shines medicinal material solution in pairs with legal system.According to the thin-layered chromatography test, draw need testing solution 10～20 μ l, control medicinal material solution 5～15 μ l, put respectively on same thin layer plate, with toluene-ethyl acetate-formic acid (21～7: 6～2: 0.75～0.25) be developping agent, launch, take out, dry, put under the uviol lamp and inspect.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color;
The qualitative identification of the fleece-flower root comprises the following steps: to get 10～20 of infantile health-care capsule chewable tablets, grinds, and adds water saturated normal butyl alcohol 25～75ml, reflux 0.5～1.5 hour filters the filtrate evaporate to dryness, residue adds methyl alcohol 0.5～1.5ml makes dissolving, as need testing solution.Other gets fleece-flower root control medicinal material 0.5～1.5g, grinds, and adds water saturated normal butyl alcohol 10～30ml, shines medicinal material solution in pairs with legal system.According to the thin-layered chromatography test, draw each 5～15 μ l of above-mentioned two kinds of solution, put respectively on same thin layer plate, with benzene-acetone-methyl alcohol (9～3: 3～1: 1.5～0.5) be developping agent, launch, take out, dry, spray is with the phosphomolybdic acid sulfuric acid solution, and it is clear to be heated to spot colour developing at 105 ℃.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color;
The qualitative identification of dried orange peel comprises the following steps: to get 10～20 of infantile health-care capsule chewable tablets, grinds, and adds ethyl acetate 25～75ml, and sonicated 20～60 minutes filters, and filtrate evaporate to dryness, residue add methyl alcohol 1～2ml makes dissolving, as need testing solution.Other gets the aurantiamarin reference substance, adds methyl alcohol and makes the solution that every 1ml contains 1～3mg, in contrast product solution.Test according to thin-layered chromatography, draw need testing solution 10～20 μ l, reference substance solution 5～15 μ l, put respectively on same thin layer plate, (48～16: 25.5～8.5: lower floor's solution 7.5～2.5) is developping agent, launches with methenyl choloride-methanol-water, take out, dry, spray is put under the uviol lamp and is inspected with 1～3% aluminium choride methanol solution.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the fluorescence spot of same color;
The b assay: the Determination of Hesperidin Content assay method comprises the following steps:
According to high performance liquid chromatography
The test of chromatographic condition and system suitability is a filling agent with octadecylsilane chemically bonded silica or octyl group silane group silica gel or cyano group or amino bonded silica gel, with acetonitrile-0.1% phosphoric acid solution (25～15: 85～75) be moving phase, the detection wavelength is 250～350nm, and number of theoretical plate calculates by the aurantiamarin peak should be not less than 2000～4000;
It is an amount of that the aurantiamarin reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds methyl alcohol and makes the solution that every 1ml contains 10～20 μ g, promptly;
5～15 of infantile health-care capsule chewable tablets are got in the preparation of need testing solution, and accurate the title decides, and porphyrize is got about 0.5～1.5g, the accurate title, decide, and puts in the tool plug conical flask, accurate methyl alcohol 25～75ml, the close plug of adding, claim decide weight, sonicated 20～60 minutes is put coldly, and weight decided in title again, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, precision is measured subsequent filtrate 1～3ml, put in the 10ml measuring bottle, be diluted to scale, shake up with methyl alcohol, filter with miillpore filter (0.45 μ m), get subsequent filtrate, promptly;
Accurate respectively reference substance solution and each 5～15 μ l of need testing solution of drawing of determination method inject liquid chromatograph, measure, promptly;
Every of infantile health-care capsule chewable tablets contains dried orange peel with aurantiamarin (C
28H
34O
15) meter, must not be less than 1.5mg.
A discrimination method in this method and b content assaying method are one or more of following method:
15 of infantile health-care capsule chewable tablets are got in the discriminating of Radix Codonopsis, grind, and add ethanol 50ml, sonicated 30 minutes filters, and filtrate volatilizes, residue adds water 30ml makes dissolving, adds hydrochloric acid 2ml, methenyl choloride 30ml, reflux 40 minutes, put coldly, divide and to get methenyl choloride liquid, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution.Other gets Radix Codonopsis control medicinal material 1g, shines medicinal material solution in pairs with legal system.Test according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution 15 μ l, control medicinal material solution 10 μ l, put respectively on same silica gel g thin-layer plate, with toluene-ethyl acetate-formic acid (14: 4: 0.5) is developping agent, launches, and takes out, dry, put under the uviol lamp (365nm) and inspect.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color;
15 of infantile health-care capsule chewable tablets are got in the discriminating of the fleece-flower root, grind, and add water saturated normal butyl alcohol 50ml, and reflux 1 hour filters, and filtrate evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution.Other gets fleece-flower root control medicinal material 1g, grinds, and adds water saturated normal butyl alcohol 20ml, shines medicinal material solution in pairs with legal system.Test according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with benzene-acetone-methyl alcohol (6: 2: 1) is developping agent, launch, take out, dry, spray is with the phosphomolybdic acid sulfuric acid solution, and it is clear to be heated to the spot colour developing at 105 ℃.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color;
15 of infantile health-care capsule chewable tablets are got in the discriminating of dried orange peel, grind, and add ethyl acetate 50ml, and sonicated 40 minutes filters, and filtrate evaporate to dryness, residue add methyl alcohol 1～2ml makes dissolving, as need testing solution.Other gets the aurantiamarin reference substance, adds methyl alcohol and makes the solution that every 1ml contains 2mg, in contrast product solution.Test according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution 15 μ l, reference substance solution 10 μ l, putting respectively on same silica gel g thin-layer plate, is developping agent with lower floor's solution of methenyl choloride-methanol-water (32: 17: 5), launches, take out, dry, spray is put under the uviol lamp (365nm) and is inspected with 2% aluminium choride methanol solution.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the fluorescence spot of same color;
B assay Determination of Hesperidin Content is measured
According to high performance liquid chromatography
Chromatographic condition and system suitability test are filling agent with the octadecylsilane chemically bonded silica, are moving phase with acetonitrile-0.1% phosphoric acid solution (20: 80), and the detection wavelength is 283nm, and number of theoretical plate calculates by the aurantiamarin peak should be not less than 3000;
It is an amount of that the aurantiamarin reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds methyl alcohol and makes the solution that every 1ml contains 15 μ g, promptly;
10 of infantile health-care capsule chewable tablets are got in the preparation of need testing solution, and accurate the title decides, and porphyrize is got about 1g, the accurate title, decide, and puts in the tool plug conical flask, accurate methyl alcohol 50ml, the close plug of adding, claim to decide weight, sonicated (power 150W, frequency 40kHz) 40 minutes is put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up, filter with methyl alcohol, precision is measured subsequent filtrate 2ml, puts in the 10ml measuring bottle, is diluted to scale with methyl alcohol, shakes up, filter with miillpore filter (0.45 μ m), get subsequent filtrate, promptly;
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of determination method inject liquid chromatograph, measure, promptly;
Every of infantile health-care capsule chewable tablets contains dried orange peel with aurantiamarin (C
28H
34O
15) meter, must not be less than 1.5mg.
Beneficial effect of the present invention: the present invention has formulated thin-layer chromatography through test of many times and has differentiated and the assay project in the quality standard of this kind, provide infantile health-care capsule chewable tablets quality inspection method and standard, by setting up strong discriminating of clear and definite specificity and reappearance, the content assaying method that stability and precision are good, can effectively control the quality of infantile health-care capsule chewable tablets, make infantile health-care capsule chewable tablets quality reach stable, controlled, the efficient safety that reaches, be that feeding intake of product required and the quality control strictness, overcome the deficiencies in the prior art, improve the quality of product, curative effect, bioavilability, the product quality height, can guarantee the product curative effect, satisfy the needs of medical treatment better.
Description of drawings:
Fig. 1 is that the thin-layer chromatography of Radix Codonopsis of the present invention is differentiated;
Fig. 2 is that the thin-layer chromatography of the fleece-flower root of the present invention is differentiated;
Fig. 3 is that the thin-layer chromatography of dried orange peel of the present invention is differentiated;
Fig. 4 is the high-efficient liquid phase chromatogram of aurantiamarin reference substance of the present invention;
Fig. 5 is the high-efficient liquid phase chromatogram of infantile health-care capsule chewable tablets test sample of the present invention;
Fig. 6 is the high-efficient liquid phase chromatogram of negative control of the present invention;
Fig. 7 is an aurantiamarin canonical plotting of the present invention;
Fig. 8 is the high-efficient liquid phase chromatogram of the lot number 20050116 of assay of the present invention;
Fig. 9 is the high-efficient liquid phase chromatogram of the lot number 20050117 of assay of the present invention;
Figure 10 is the high-efficient liquid phase chromatogram of the lot number 20050118 of assay of the present invention;
Figure 11 is the high-efficient liquid phase chromatogram of the lot number 20050312 of assay of the present invention;
Figure 12 is the high-efficient liquid phase chromatogram of the lot number 20050315 of assay of the present invention;
Figure 13 is the high-efficient liquid phase chromatogram of the lot number 20050316 of assay of the present invention;
Embodiment:
Embodiment:
A kind of infantile health-care capsule chewable tablets quality standard and the method for inspection thereof, the quality standard of this tablet kind comprise characteristic index, thin-layer chromatography identification beacon, assay index, and described every index is as follows:
(1). characteristic index: the infantile health-care capsule chewable tablets is brown or tan; Gas perfume (or spice), it is sweet to distinguish the flavor of;
(2). thin-layer chromatography identification beacon: in the test sample chromatogram, answer the blob features of tool codonopsis pilosula, dried orange peel, fleece-flower root medicinal material;
(3). the assay index: every of infantile health-care capsule chewable tablets contains dried orange peel with aurantiamarin (C
28H
34O
15) meter, must not be less than 1.5mg.
The method of inspection of quality standard of the present invention is: (1) proterties: adopt range estimation, nasil and mouth to taste: (2) thin-layer chromatography is differentiated: adopt thin-layered chromatography; (3) assay: adopt high performance liquid chromatography.
The said thin-layer chromatography identification of test method of the present invention is:
1. the qualitative identification of wherein said Radix Codonopsis comprises the following steps: to get 10～20 of infantile health-care capsule chewable tablets, grinds, and adds ethanol 25～75ml, sonicated or hot reflux 15～45 minutes filter, and filtrate volatilizes, residue adds water 15～45ml makes dissolving, adds hydrochloric acid 1～3ml, methenyl choloride 15～45ml, reflux 20～60 minutes, put coldly, divide and to get methenyl choloride liquid, evaporate to dryness, residue adds methyl alcohol 0.5～1.5ml makes dissolving, as need testing solution.Other gets Radix Codonopsis control medicinal material 0.5～1.5g, shines medicinal material solution in pairs with legal system.According to the thin-layered chromatography test, draw need testing solution 10～20 μ l, control medicinal material solution 5～15 μ l, put respectively on same thin layer plate, with toluene-ethyl acetate-formic acid (21～7: 6～2: 0.75～0.25) be developping agent, launch, take out, dry, put under the uviol lamp and inspect.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.See Fig. 1.
2. the qualitative identification of the wherein said fleece-flower root comprises the following steps: to get 10～20 of infantile health-care capsule chewable tablets, grinds, and adds water saturated normal butyl alcohol 25～75ml, reflux 0.5～1.5 hour filters the filtrate evaporate to dryness, residue adds methyl alcohol 0.5～1.5ml makes dissolving, as need testing solution.Other gets fleece-flower root control medicinal material 0.5～1.5g, grinds, and adds water saturated normal butyl alcohol 10～30ml, shines medicinal material solution in pairs with legal system.According to the thin-layered chromatography test, draw each 5～15 μ l of above-mentioned two kinds of solution, put respectively on same thin layer plate, with benzene-acetone-methyl alcohol (9～3: 3～1: 1.5～0.5) be developping agent, launch, take out, dry, spray is with the phosphomolybdic acid sulfuric acid solution, and it is clear to be heated to spot colour developing at 105 ℃.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color.See Fig. 2.
3. the qualitative identification of wherein said dried orange peel comprises the following steps: to get 10～20 of infantile health-care capsule chewable tablets, grinds, and adds ethyl acetate 25～75ml, and sonicated 20～60 minutes filters, and filtrate evaporate to dryness, residue add methyl alcohol 1～2ml makes dissolving, as need testing solution.Other gets the aurantiamarin reference substance, adds methyl alcohol and makes the solution that every 1ml contains 1～3mg, in contrast product solution.Test according to thin-layered chromatography, draw need testing solution 10～20 μ l, reference substance solution 5～15 μ l, put respectively on same thin layer plate, (48～16: 25.5～8.5: lower floor's solution 7.5～2.5) is developping agent, launches with methenyl choloride-methanol-water, take out, dry, spray is put under the uviol lamp and is inspected with 1～3% aluminium choride methanol solution.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the fluorescence spot of same color.See Fig. 3.
(2) assay Determination of Hesperidin Content assay method comprises the following steps:
According to high performance liquid chromatography
The test of chromatographic condition and system suitability is a filling agent with octadecylsilane chemically bonded silica or octyl group silane group silica gel or cyano group or amino bonded silica gel; (25～15: 85～75) be moving phase, the detection wavelength is 250～350nm with acetonitrile-0.1% phosphoric acid solution.Number of theoretical plate calculates by the aurantiamarin peak should be not less than 2000～4000.
It is an amount of that the aurantiamarin reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds methyl alcohol and makes the solution that every 1ml contains 10～20 μ g, promptly.
5～15 of infantile health-care capsule chewable tablets are got in the preparation of need testing solution, and accurate the title decides, and porphyrize is got about 0.5～1.5g, the accurate title, decide, and puts in the tool plug conical flask, accurate methyl alcohol 25～75ml, the close plug of adding, claim decide weight, sonicated 20～60 minutes is put coldly, and weight decided in title again, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, precision is measured subsequent filtrate 1～3ml, put in the 10ml measuring bottle, be diluted to scale, shake up with methyl alcohol, filter with miillpore filter (0.45 μ m), get subsequent filtrate, promptly.
Accurate respectively reference substance solution and each 5～15 μ l of need testing solution of drawing of determination method inject liquid chromatograph, measure, promptly.
Every of infantile health-care capsule chewable tablets contains dried orange peel with aurantiamarin (C
28H
34O
15) meter, must not be less than 1.5mg.
1. instrument and reagent
1.1 instrument: Agilent-1100 chem workstation, UV-detector
Apollo C
185u (4.6 * 250mm) chromatographic columns
1.2 reagent and reagent: the aurantiamarin reference substance (for assay with) provide by Nat'l Pharmaceutical ﹠ Biological Products Control Institute that (lot number is: 0721-9909).Acetonitrile is a chromatographically pure, and water is high purity water, and other reagent is pure for analyzing.
1.3 sample: provide by Baotou Chinese Traditional Medicine Co., Ltd..
2. selection of experiment conditions
2.1 the investigation of extracting method: with reference to relevant Determination of Hesperidin Content assay method in one one of the Chinese Pharmacopoeia version in 2000, compared ultrasonic method and Soxhlet reflux extraction, the result shows, two kinds of methods record basically identical as a result, be handled easily, save time, so selected ultrasonic extraction.
Determining of ultrasonic time: investigated sonicated respectively 20,30,40,50 minutes, the result shows, sonicated 40 minutes, and content no longer increases, so determine sonicated 40 minutes.
2.2 the selection of chromatographic condition
The selection of moving phase: with reference to the relevant Determination of Hesperidin Content assay method that records in one one of the Chinese Pharmacopoeia version in 2000, methanol-water (35: 65), methyl alcohol-0.1% acetum (40: 60), acetonitrile-0.2% phosphoric acid solution (20: 80), acetonitrile-0.1% phosphoric acid solution moving phases such as (20: 80) have been compared, the result shows: acetonitrile-0.1% phosphoric acid solution (20: 80) is a moving phase, appearance time is moderate, the chromatographic peak peak shape is more satisfactory, baseline is steady, and degree of separation is good.So selecting acetonitrile-0.1% phosphoric acid solution (20: 80) is moving phase.
Detect the selection of wavelength: prove according to documents and materials report and ultraviolet absorpting spectrum: the aurantiamarin maximum absorption wavelength is 283nm, so detect wavelength selective 2 83nm.
Chromatographic condition: Apollo C
18Post (250mm * 4.6,5 μ m); Moving phase is acetonitrile-0.1% phosphoric acid solution (20: 80); Flow velocity is 1.0ml/min, and the detection wavelength is 283nm.
Under above-mentioned selected chromatographic condition, the degree of separation at aurantiamarin and last peak is greater than 1.5, and greater than 3000, and negative sample is noiseless by the aurantiamarin peak for number of theoretical plate.See Fig. 4, Fig. 5, Fig. 6.
3. methodological study
3.1 linear relationship is investigated
It is an amount of to get the aurantiamarin reference substance, and accurate the title decides, and adds methyl alcohol and makes the solution that every 1ml contains 14.32 μ g, in contrast product solution.Above-mentioned reference substance solution 6,8,10,12,14, the 16 μ l of accurate absorption, inject liquid chromatograph, measure by above-mentioned chromatographic condition, with sample size peak area value is carried out regretional analysis, aurantiamarin presents good linear relationship in 0.0859～0.2291 μ g scope as a result.Regression equation is: A=1567.1C+1.5014, r=0.9999.The results are shown in Table 3, Fig. 7.
Table 1 standard curve determination result
| Sample size (μ g) | 0.0859 0.1146 0.1432 0.1718 0.2005 0.2291 |
| Peak area | 135.18 182.05 227.33 269.07 315.56 360.86 |
3.2 stability test
Get same lot number test sample, be equipped with need testing solution by [assay] below legal system, respectively at 0,2,4,6,8 hour difference sample introduction, record aurantiamarin peak area integrated value, and try to achieve content, the results are shown in Table 2.
Table 2 stability test is table as a result
| Time | Peak area | Content (mg/ sheet) | Average content (mg/ sheet) | RSD(％) |
| 0 2 4 6 8 | 277.470 277.577 274.590 279.989 280.318 | 2.33 2.33 2.31 2.35 2.35 | 2.33 | 0.7 |
The result shows: this product measurement result in 8 hours is stable.
3.3 precision test
Get same lot number test sample, be equipped with need testing solution by [assay] below legal system, continuous sample introduction 5 times, measurement result sees Table 3.
Table 3 Precision test result
| Sequence number | Peak area | Content (mg/ sheet) | Average content (mg/ sheet) | RSD(％) |
| 1 2 3 4 5 | 279.350 282.490 282.239 278.215 276.010 | 2.35 2.37 2.37 2.34 2.32 | 2.35 | 0.9 |
The result shows: this law precision is up to specification.
3.4 replica test
Get 5 parts of same lot number test samples, press [assay] following method operation respectively and measure every part of content, the results are shown in Table 4.
Table 4 replica test result
| Sequence number | Sample weighting amount (g) | Peak area | Content (mg/ sheet) | Average content (mg/ sheet) | RSD(％) |
| 1 2 | 1.0027 1.0176 | 274.590 281.922 | 2.31 2.33 |
[0097]
| 3 4 5 | 1.0030 1.0062 1.0028 | 261.628 277.470 262.250 | 2.20 2.33 2.21 | 2.27 | 2.8 |
The result shows that this law repeatability better.
3.5 recovery test
Get 5 parts of the same test samples of known content, every part of 0.5g accurately claims surely, and accurate respectively aurantiamarin reference substance solution (0.328mg/ml) 5ml that adds is by [assay] down method operation and measure every part content, calculate recovery rate.The results are shown in Table 5.
Table 5 average recovery test findings
| Sequence number | Sampling amount (g) | Peak area | Sample size (mg/g) | Addition (mg) | The amount of recording (mg) | The recovery (%) | Average recovery rate (%) | RSD(％) |
| 1 2 3 4 5 | 0.5040 0.5009 0.5022 0.5019 0.5003 | 249.339 244.850 247.866 248.816 244.657 | 3.56 3.56 3.56 3.56 3.56 | 1.64 1.64 1.64 1.64 1.64 | 1.647 1.596 1.633 1.647 1.595 | 100.42 97.31 99.57 100.42 97.25 | 98.99 | 1.6 |
The result shows: this law recovery is up to specification.
3.6 the mensuration of sample
Get the about 1g of different lot number samples respectively, the accurate title, decide, and presses [assay] item method operation and mensuration down, the results are shown in Table 6.
Table 6 sample determination result
| Lot number | Sample size (g) | Peak area | Content (mg/ sheet) |
| 20050116 20050117 20050118 20050312 20050315 20050316 | 1.0152 1.0229 1.0096 1.0178 1.0292 1.0201 | 276.761 280.408 274.051 277.730 276.558 271.211 | 2.34 2.34 2.33 2.37 2.30 2.27 |
According to above 6 batch sample assay results, tentative every of this product contains dried orange peel with aurantiamarin (C
28H
34O
15) meter, must not be advisable less than 1.5mg.See Fig. 8～13.
In order to investigate the steadiness that quality standard improves back infantile health-care capsule chewable tablets, carried out the stability test that keeps sample of accelerated stability and room temperature:
1. experiment condition:
(1), the room temperature investigation method that keeps sample: sample thief, under the listing terms of packing, put under the room temperature condition and investigate, the results are shown in Table 7～9.
(2), accelerated stability experimental method: it is to investigate under 40 ℃ ± 2 ℃, the condition of relative humidity 75% ± 5% that sample is placed temperature, the results are shown in Table 10～12.
2. investigation result
(1), this product transfers through normal temperature and put reserved sample observing 6 months, its every detection index and initial of that month check result all do not have obvious change, every index is up to specification.Room temperature is placed the long-time stability experiment and is remained to be proceeded.
(2), this product experiment showed, under this experiment condition that through accelerated stability its every detection index and initial of that month assay all do not have obvious change.
The subordinate list 7 room temperatures investigation result that keeps sample
Sample title: infantile health-care capsule chewable tablets
Lot number: 20050312
| Experimental period project, standard code, |
0 month 2005. 3 | 1 month 2005. 4 | 2 months 2005. 5 | 3 months 2005. 6 | 6 months 2005. 9 | |
| Proterties | The infantile health-care capsule chewable tablets is brown or tan; Gas perfume (or spice), it is sweet to distinguish the flavor of. | Qualified | Qualified | Qualified | Qualified | Qualified |
| Differentiate | Radix Codonopsis | Qualified | Qualified | Qualified | Qualified | Qualified |
| Dried orange peel | Qualified | Qualified | Qualified | Qualified | Qualified | |
| The fleece-flower root | Qualified | Qualified | Qualified | Qualified | Qualified | |
| Check | In weight differential ± 5% | Qualified | Qualified | Qualified | Qualified | Qualified |
| Assay (mg/ sheet) | Every contains dried orange peel with aurantiamarin (C 28H 34O 15) meter, must not be less than 1.5mg. | 2.37 | 2.35 | 2.37 | 2.38 | 2.36 |
| Microbial limit | Total number of bacteria must not be crossed 1000/g total number of molds and must not cross 100/g Escherichia coli and must not detect | ＜10＜10 do not detect | ＜10＜10 do not detect | ＜10＜10 do not detect | ＜10＜10 do not detect | ＜10＜10 do not detect |
The result: room temperature was placed 6 months, and every detection index is all up to specification.
The subordinate list 8 room temperatures investigation result that keeps sample
Sample title: infantile health-care capsule chewable tablets
Lot number: 20050315
| Experimental period project, standard code, |
0 month 2005. 3 | 1 month 2005. 4 | 2 months 2005. 5 | 3 months 2005. 6 | 6 months 2005. 9 | |
| Proterties | The infantile health-care capsule chewable tablets is brown or tan; Gas perfume (or spice), it is sweet to distinguish the flavor of. | Qualified | Qualified | Qualified | Qualified | Qualified |
| Differentiate | Radix Codonopsis | Qualified | Qualified | Qualified | Qualified | Qualified |
| Dried orange peel | Qualified | Qualified | Qualified | Qualified | Qualified | |
| The fleece-flower root | Qualified | Qualified | Qualified | Qualified | Qualified | |
| Check | In weight differential ± 5% | Qualified | Qualified | Qualified | Qualified | Qualified |
| Assay (mg/ sheet) | Every contains dried orange peel with aurantiamarin (C 28H 34O 15) meter, must not be less than 1.5mg. | 2.30 | 2.22 | 2.23 | 2.29 | 2.28 |
| Microbial limit | Total number of bacteria must not be crossed 1000/g total number of molds and must not cross 100/g Escherichia coli and must not detect | ＜10＜10 do not detect | ＜10＜10 do not detect | ＜10＜10 do not detect | ＜10＜10 do not detect | ＜10＜10 do not detect |
The result: room temperature was placed 6 months, and every detection index is all up to specification.
The subordinate list 9 room temperatures investigation result that keeps sample
Sample title: infantile health-care capsule chewable tablets
Lot number: 20050316
| Experimental period project, standard code, |
0 month 2005. 3 | 1 month 2005. 4 | 2 months 2005. 5 | 3 months 2005. 6 | 6 months 2005. 9 | |
| Proterties | The infantile health-care capsule chewable tablets is brown or tan; Gas perfume (or spice), it is sweet to distinguish the flavor of. | Qualified | Qualified | Qualified | Qualified | Qualified |
| Differentiate | Radix Codonopsis | Qualified | Qualified | Qualified | Qualified | Qualified |
| Dried orange peel | Qualified | Qualified | Qualified | Qualified | Qualified | |
| The fleece-flower root | Qualified | Qualified | Qualified | Qualified | Qualified | |
| Check | In weight differential ± 5% | Qualified | Qualified | Qualified | Qualified | Qualified |
| Assay (mg/ sheet) | Every contains dried orange peel with aurantiamarin (C 28H 34O 15) meter, must not be less than 1.5mg. | 2.27 | 2.31 | 2.31 | 2.31 | 2.32 |
| Microbial limit | Total number of bacteria must not be crossed 1000/g total number of molds and must not cross 100/g Escherichia coli and must not detect | ＜10＜10 do not detect | ＜10＜10 do not detect | ＜10＜10 do not detect | ＜10＜10 do not detect | ＜10＜10 do not detect |
The result: room temperature was placed 6 months, and every detection index is all up to specification.
Sample title: infantile health-care capsule chewable tablets
Lot number: 20050312
| Experimental period project, standard code, |
0 month 2005. 3 | 1 month 2005. 4 | 2 months 2005. 5 | 3 months 2005. 6 | |
| Proterties | The infantile health-care capsule chewable tablets is brown or tan; Gas perfume (or spice), it is sweet to distinguish the flavor of. | Qualified | Qualified | Qualified | Qualified |
| Differentiate | Radix Codonopsis | Qualified | Qualified | Qualified | Qualified |
| Dried orange peel | Qualified | Qualified | Qualified | Qualified | |
| The fleece-flower root | Qualified | Qualified | Qualified | Qualified | |
| Check | In weight differential ± 5% | Qualified | Qualified | Qualified | Qualified |
| Assay (mg/ sheet) | Every contains dried orange peel with aurantiamarin (C 28H 34O 15) meter, must not be less than 1.5mg. | 2.37 | 2.36 | 2.35 | 2.37 |
| Microbial limit | Total number of bacteria must not be crossed 1000/g total number of molds and must not cross 100/g Escherichia coli and must not detect | ＜10＜10 do not detect | ＜10＜10 do not detect | ＜10＜10 do not detect | ＜10＜10 do not detect |
The result: accelerated test 3 months, every detection index is all up to specification.
Subordinate list 11 accelerated tests are investigated the result
Sample title: infantile health-care capsule chewable tablets
Lot number: 20050315
| Experimental period project, standard code, |
0 month 2005. 3 | 1 month 2005. 4 | 2 months 2005. 5 | 3 months 2005. 6 | |
| Proterties | The infantile health-care capsule chewable tablets is brown or tan; Gas perfume (or spice), it is sweet to distinguish the flavor of. | Qualified | Qualified | Qualified | Qualified |
| Differentiate | Radix Codonopsis | Qualified | Qualified | Qualified | Qualified |
| Dried orange peel | Qualified | Qualified | Qualified | Qualified | |
| The fleece-flower root | Qualified | Qualified | Qualified | Qualified | |
| Check | In weight differential ± 5% | Qualified | Qualified | Qualified | Qualified |
| Assay (mg/ sheet) | Every contains dried orange peel with aurantiamarin (C 28H 34O 15) meter, must not be less than 1.5mg. | 2.30 | 2.26 | 2.29 | 2.24 |
| Microbial limit | Total number of bacteria must not be crossed 1000/g total number of molds and must not cross 100/g Escherichia coli and must not detect | ＜10＜10 do not detect | ＜10＜10 do not detect | ＜10＜10 do not detect | ＜10＜10 do not detect |
The result: accelerated test 3 months, every detection index is all up to specification.
Subordinate list 12 accelerated tests are investigated the result
Sample title: infantile health-care capsule chewable tablets
Lot number: 20050316
| Experimental period project, standard code, |
0 month 2005. 3 | 1 month 2005. 4 | 2 months 2005. 5 | 3 months 2005. 6 | |
| Proterties | The infantile health-care capsule chewable tablets is brown or tan; Gas perfume (or spice), it is sweet to distinguish the flavor of. | Qualified | Qualified | Qualified | Qualified |
| Differentiate | Radix Codonopsis | Qualified | Qualified | Qualified | Qualified |
| Dried orange peel | Qualified | Qualified | Qualified | Qualified | |
| The fleece-flower root | Qualified | Qualified | Qualified | Qualified | |
| Check | In weight differential ± 5% | Qualified | Qualified | Qualified | Qualified |
| Assay (mg/ sheet) | Every contains dried orange peel with aurantiamarin (C 28H 34O 15) meter, must not be less than 1.5mg. | 2.27 | 2.34 | 2.31 | 2.32 |
| Microbial limit | Total number of bacteria must not be crossed 1000/g total number of molds and must not cross 100/g Escherichia coli and must not detect | ＜10＜10 do not detect | ＜10＜10 do not detect | ＜10＜10 do not detect | ＜10＜10 do not detect |
The result: accelerated test 3 months, every detection index is all up to specification.
Beneficial effect of the present invention: the present invention has formulated thin-layer chromatography through test of many times and has differentiated and the assay project in the quality standard of this kind. The present invention just provides infantile health-care capsule chewable tablets quality inspection method and standard. The present invention can effectively control the quality of infantile health-care capsule chewable tablets by setting up the strong discriminating of specificity and the good content assaying method of reappearance, stability and precision, makes the quality of infantile health-care capsule chewable tablets reach stable, controlled, efficiently reach safety.
Claims (2)
1. the method for inspection of an infantile health-care capsule chewable tablets, it is characterized in that: the content assaying method in this method is a kind of of following method:
Assay: the Determination of Hesperidin Content assay method comprises the following steps:
According to high performance liquid chromatography
The test of chromatographic condition and system suitability is a filling agent with octadecylsilane chemically bonded silica or octyl group silane group silica gel or cyano group or amino bonded silica gel, with acetonitrile-0.1% phosphoric acid solution 25～15: 85～75 is moving phase, the detection wavelength is 250～350nm, and number of theoretical plate calculates by the aurantiamarin peak should be not less than 2000～4000;
It is an amount of that the aurantiamarin reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds methyl alcohol and makes the solution that every 1ml contains 10～20 μ g, promptly;
5～15 of infantile health-care capsule chewable tablets are got in the preparation of need testing solution, and accurate the title decides, and porphyrize is got about 0.5～1.5g, the accurate title, decide, and puts in the tool plug conical flask, accurate methyl alcohol 25～75ml, the close plug of adding, claim decide weight, sonicated 20～60 minutes is put coldly, and weight decided in title again, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, precision is measured subsequent filtrate 1～3ml, put in the 10ml measuring bottle, be diluted to scale, shake up with methyl alcohol, filter with miillpore filter 0.45 μ m, get subsequent filtrate, promptly;
Accurate respectively reference substance solution and each 5～15 μ l of need testing solution of drawing of determination method inject liquid chromatograph, measure, promptly.
2. method according to claim 1, a kind of method of inspection of infantile health-care capsule chewable tablets is characterized in that: the content assaying method in this method is a kind of of following method:
The assay Determination of Hesperidin Content is measured
According to high performance liquid chromatography
Chromatographic condition and system suitability test are filling agent with the octadecylsilane chemically bonded silica, are at 20: 80 moving phase with acetonitrile-0.1% phosphoric acid solution, and the detection wavelength is 283nm, and number of theoretical plate calculates by the aurantiamarin peak should be not less than 3000;
It is an amount of that the aurantiamarin reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds methyl alcohol and makes the solution that every 1ml contains 15 μ g, promptly;
10 of infantile health-care capsule chewable tablets are got in the preparation of need testing solution, and accurate the title decides, and porphyrize is got about 1g, the accurate title, decide, and puts in the tool plug conical flask, accurate methyl alcohol 50ml, the close plug of adding, claim to decide weight, sonicated power 150W frequency 40kHz40 minute, is put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up, filter with methyl alcohol, precision is measured subsequent filtrate 2ml, puts in the 10ml measuring bottle, is diluted to scale with methyl alcohol, shakes up, filter with miillpore filter 0.45 μ m, get subsequent filtrate, promptly;
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of determination method inject liquid chromatograph, measure, promptly.
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| CN1951491A (en) * | 2006-08-16 | 2007-04-25 | 湖南科威制药有限公司 | Method for preparing blood replenishing capsule 'Wei Xue Kang' |
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| CN1951491A (en) * | 2006-08-16 | 2007-04-25 | 湖南科威制药有限公司 | Method for preparing blood replenishing capsule 'Wei Xue Kang' |
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| 中华人民共和国卫生部药典委员会.中华人民共和国药品标准×中药成方制剂 14.中华人民共和国卫生部药典委员会,1997,168. * |
| 中华人民共和国卫生部药典委员会.中华人民共和国药品标准×中药成方制剂14.中华人民共和国卫生部药典委员会,1997,168. |
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