CN102218122A - Quality control and detection method for sea dragon and gecko oral liquid - Google Patents

Quality control and detection method for sea dragon and gecko oral liquid Download PDF

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CN102218122A
CN102218122A CN2011100920838A CN201110092083A CN102218122A CN 102218122 A CN102218122 A CN 102218122A CN 2011100920838 A CN2011100920838 A CN 2011100920838A CN 201110092083 A CN201110092083 A CN 201110092083A CN 102218122 A CN102218122 A CN 102218122A
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solution
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liquid
water
gecko
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CN102218122B (en
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李樱
刘圣梅
姜广玲
秦秀玲
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SHANDONG HONGJITANG PHARMACEUTICAL GROUP CO., LTD.
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HONGJITANG PHARMACY CO Ltd JINAN
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Abstract

The invention discloses a quality control and detection method for a sea dragon and gecko oral liquid. In the quality control and detection method, on the basis of the original detection standard, a thin-layer chromatography detection method for dried tangerine or orange peel and astragalus root in the prescription of the sea dragon and gecko oral liquid is added, a thin-layer chromatography for ginseng and the astragalus root is improved, and a high performance liquid chromatography for measuring the content of epimedim herb of in the prescription is added. The detection project designed by the invention is reasonable; and the detection method provided by the invention has the advantages of advancement and good accuracy and repeatability, is used for carrying out the quality control on the sea dragon and gecko oral liquid, and can carry out the comprehensive quality control on the sea dragon and gecko oral liquid to ensure the stability and uniformity of product quality.

Description

A kind of quality control detection method of Solenognathus Gecko oral liquid
Technical field
The invention discloses a kind of warming the kidney to invigorate YANG that has, the quality control detection method of the Solenognathus Gecko oral liquid of enrich and benefit essence and blood effect.
Background technology
" Solenognathus Gecko oral liquid " function cures mainly: warming the kidney to invigorate YANG, enrich and benefit essence and blood.It is aching and limp to be used for the waist foot, and the complexion white light is white, impotence and seminal emission, and cold womb is infertile, the vertigo.
The former examination criteria of " Solenognathus Gecko oral liquid " records in the 13 in Drug Standard of Ministry of Public Health of the Peoples Republic of China Chinese traditional patent formulation preparation.Have only the thin layer chromatography of medical material Radix Ginseng and Radix Scutellariae to differentiate that because the test item of primary standard is few, method is single in the primary standard, therefore can not guarantee the quality of this medicine is comprehensively controlled and detected.
Summary of the invention
The invention provides the quality control detection method of Solenognathus Gecko oral liquid, the quality control that is used for Solenognathus Gecko oral medicine liquid, the test item of the present invention's design is reasonable, the detection method advanced person who provides, precision and favorable reproducibility, can comprehensively carry out quality control, guarantee the stable homogeneity of product quality Solenognathus Gecko oral liquid.
The quality control detection method of Solenognathus Gecko oral liquid of the present invention, with Solenognathus 39.1g, Gecko 0.73g, Radix Ginseng 4.68g, Testis Et penis Caprae seu Ovis 4.68g, Testis Caprae seu Ovis 4.68g, Radix Scutellariae 4.68g, Radix Rehmanniae Preparata 3.1g, Semen Cuscutae 3.1g, Radix Polygoni Multiflori 3.1g, Radix Rehmanniae 3.1g, Pericarpium Citri Reticulatae 3.1g, Radix Angelicae Sinensis 1.56g, Radix Astragali 4.68g, Actinolitum 1.56g, Stamen Nelumbinis 1.56g, Radix Glycyrrhizae 1.56g, Rhizoma Chuanxiong 1.56g, Rhizoma Alismatis 1.56g, Herba Cynomorii 1.56g, Fructus Amomi Rotundus 1.56g, Lignum Aquilariae Resinatum 1.56g, Cornu Cervi Pantotrichum 1.56g, Fructus Lycii 1.56g, Herba Cistanches 0.78g, Adeps Caprae seu ovis Herba Epimedii Preparata 1.56g, Cortex Cinnamomi 1.56g, Semen Allii Tuberosi 1.56g, Fructus Cnidii 1.56g, Pericarpium Zanthoxyli 0.31g 29 flavor compositions decoct with water secondary, each 2 hours, collecting decoction, being concentrated into relative density at 80 ℃ is 1.04~1.06 clear paste, add the ethanol qdx, cold preservation 12 hours, filter, concentrate, add water, cold preservation, filter, filtrate adds benzoic acid makes dissolving in right amount, transfer pH value 4.6~4.8 with 8% sodium hydroxide, add correctives xylitol 3%, adjust total amount to 1000ml, filter, packing, sterilization, promptly.Light brown is to the liquid of rufous; Mildly bitter flavor.
The quality control detection method of Solenognathus Gecko oral liquid of the present invention, 1) gets Solenognathus Gecko oral liquid 30ml, 20ml adds diethyl ether, jolting is extracted, place, discard ether solution, water layer is with water saturated n-butanol extraction 3 times, and consumption is followed successively by 20ml, 15ml, 15ml, merge n-butyl alcohol liquid, add 4% potassium hydroxide solution 30ml washing once, discard washing liquid, the reuse n-butyl alcohol is saturated is washed to neutrality, discard water liquid, n-butyl alcohol liquid is put evaporate to dryness in the evaporating dish, and residue adds methanol 1ml makes dissolving, as need testing solution; Other gets ginsenoside Rg1's reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw need testing solution 10 μ l, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, lower floor's solution of placing below 10 ℃ with chloroform-methanol-water of 65:35:10 is developing solvent, launches, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
2) get Solenognathus Gecko oral liquid 40ml, use hcl acidifying, pH value 3~4 adds the ethyl acetate jolting and extracts 3 times, each 20ml, and combined ethyl acetate liquid is put evaporate to dryness in the evaporating dish, and residue adds methanol 1ml makes dissolving, as need testing solution; Other gets the baicalin reference substance, adds methanol and makes the solution that every 1ml contains 2mg, in contrast product solution; According to thin layer chromatography test, draw need testing solution 10 μ l, reference substance solution 5 μ l put respectively on same silica gel g thin-layer plate, are developing solvent with butyl acetate-formic acid-water of 1:1:1, launch, and take out, and dry, and spray is with 3% ferric chloride alcoholic solution.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
3) get Solenognathus Gecko oral liquid 60ml, add the ethyl acetate jolting and extract 3 times, each 40ml, combined ethyl acetate liquid is put evaporate to dryness in the evaporating dish, and residue adds ethyl acetate 0.5ml makes dissolving, as need testing solution; Other gets the Hesperidin reference substance, adds methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution; According to the thin layer chromatography test, draw need testing solution 15 μ l, reference substance solution 10 μ l, put respectively on the same silica gel g thin-layer plate that contains 0.5% sodium hydroxide, ethyl acetate-methanol-water with 100:17:13 is developing solvent, launches 5cm, and the upper solution with toluene-ethyl acetate-formic acid-water of 20:10:1:1 is developing solvent again, launch 13cm, take out, dry, spray is with the aluminum chloride test solution, put under the ultra-violet lamp and inspect, wavelength is 365nm; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
4) get Solenognathus Gecko oral liquid 60ml, add water saturated n-butyl alcohol jolting and extract 3 times, each 30ml, merge n-butyl alcohol liquid, add 1% sodium hydroxide solution jolting and extract 3 times, each 20ml discards sodium hydroxide solution, n-butanol layer adds the saturated water washing of n-butyl alcohol 3 times, each 20ml discards water liquid, and n-butyl alcohol liquid is put evaporate to dryness in the evaporating dish, residue adds methanol 0.5ml makes dissolving, as need testing solution; Other gets the astragaloside reference substance, adds methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer chromatography, draw need testing solution 10 μ l, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, lower floor's solution of placing below 10 ℃ with chloroform-ethyl acetate-methanol-water of 10:20:11:5 is developing solvent, launches, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
5) check: pH value is 4.0~5.0, and the relative density Sugarless type should be not less than 1.01; Low-sugar type should be not less than 1.05; Other should meet relevant every regulation under an appendix I of mixture Chinese Pharmacopoeia version in 2010 the J item;
6) assay: icariin is according to high effective liquid chromatography for measuring
Icariin: according to an appendix VI of Chinese Pharmacopoeia version in 2010 D high effective liquid chromatography for measuring;
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Acetonitrile-water with 25:75 is a mobile phase; The detection wavelength is 270nm, and column temperature is a room temperature.Number of theoretical plate calculates by the icariin peak should be not less than 1500;
The preparation of reference substance solution: it is an amount of that precision takes by weighing the icariin reference substance, uses dissolve with methanol, and be diluted to scale with methanol, shakes up, that is, the every 1ml of icariin contains 8 μ g;
The preparation of need testing solution: precision is measured Solenognathus Gecko oral liquid 40ml, and the jolting that adds diethyl ether is extracted 3 times, each 40ml, discard ether solution, water layer adds the water-saturated n-butanol jolting and extracts 4 times, and each 40ml merges n-butyl alcohol liquid, adding the jolting of 0.5mol/L sodium carbonate liquor extracts 3 times, each 40ml discards sodium carbonate liquor, evaporate to dryness in the n-butyl alcohol stratification evaporating dish, residue adds methanol 25ml makes dissolving, as need testing solution;
Algoscopy: accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, calculate, promptly.
It is C with the icariin molecular formula that the every 1ml of Solenognathus Gecko oral liquid contains Herba Epimedii 33H 40O 15Meter must not be less than 1.35 μ g.
Good effect of the present invention is: the thin-layered chromatography detection method that has increased Pericarpium Citri Reticulatae, the Radix Astragali in the Solenognathus Gecko oral liquid prescription on former examination criteria basis, improve the thin layer chromatography of Radix Ginseng and Radix Scutellariae, increased the high effective liquid chromatography for measuring content of Herba Epimedii in the prescription; The test item of the present invention's design is reasonable, the detection method advanced person who provides, precision and favorable reproducibility are used for the quality control of Solenognathus Gecko oral medicine liquid, can comprehensively carry out quality control, guarantee the stable homogeneity of product quality Solenognathus Gecko oral liquid.
The present invention is on the basis of former low sugar oral liquid, and innovation has increased the Sugarless type oral liquid, makes the suitable person of a lot of diabetes can take this oral liquid, has increased the indication crowd.
Description of drawings
Fig. 1: Radix Ginseng thin-layer chromatogram
1, ginsenoside's reference substance Rg1 2,3,4, three batch samples; 5, negative control
Fig. 2: Radix Scutellariae thin-layer chromatogram
1, baicalin; 2,3,4, three batch samples; 5, negative control
Fig. 3: Pericarpium Citri Reticulatae thin-layer chromatogram
1, Hesperidin; 2; 3; 4, three batch samples; 5, negative control
Fig. 4: Radix Astragali thin-layer chromatogram
1, astragaloside; 2,3,4, three batch samples; 5, negative control
Fig. 5: icariin reference substance uv absorption figure
Fig. 6: icariin reference substance canonical plotting
Fig. 7: icariin reference substance HPLC chromatogram
Fig. 8: the HPLC chromatogram of need testing solution
Fig. 9: the HPLC chromatogram of negative controls.
The specific embodiment
For the ease of understanding the present invention, especially exemplified by following examples.Its effect is understood that it is to explaination of the present invention but not to any type of restriction of the present invention.
Embodiment 1
Get Solenognathus 39.1g, Gecko 0.73g, Radix Ginseng 4.68g, Testis Et penis Caprae seu Ovis 4.68g, Testis Caprae seu Ovis 4.68g, Radix Scutellariae 4.68g, Radix Rehmanniae Preparata 3.1g, Semen Cuscutae 3.1g, Radix Polygoni Multiflori 3.1g, Radix Rehmanniae 3.1g, Pericarpium Citri Reticulatae 3.1g, Radix Angelicae Sinensis 1.56g, Radix Astragali 4.68g, Actinolitum 1.56g, Stamen Nelumbinis 1.56g, Radix Glycyrrhizae 1.56g, Rhizoma Chuanxiong 1.56g, Rhizoma Alismatis 1.56g, Herba Cynomorii 1.56g, Fructus Amomi Rotundus 1.56g, Lignum Aquilariae Resinatum 1.56g, Cornu Cervi Pantotrichum 1.56g, Fructus Lycii 1.56g, Herba Cistanches 0.78g, Herba Epimedii (Adeps Caprae seu ovis is processed) 1.56g, Cortex Cinnamomi 1.56g, Semen Allii Tuberosi 1.56g, Fructus Cnidii 1.56g, Pericarpium Zanthoxyli 0.31g 29 flavor compositions decoct with water secondary, each 2 hours, collecting decoction, being concentrated into relative density at 80 ℃ is 1.04~1.06 clear paste, add the ethanol qdx, cold preservation 12 hours, filter, concentrate, add water, cold preservation, filter, filtrate adds benzoic acid makes dissolving in right amount, transfers pH value 4.6~4.8 with 8% sodium hydroxide, add correctives xylitol 3%, adjust total amount to 1000ml, filter packing, sterilization, promptly.Its detection method comprises step:
1) get Solenognathus Gecko oral liquid 30ml, the 20ml that adds diethyl ether, jolting is extracted, place, discard ether solution, water layer is with water saturated n-butanol extraction 3 times, consumption is followed successively by 20ml, 15ml, 15ml, merges n-butyl alcohol liquid, adds 4% potassium hydroxide solution 30ml washing once, discard washing liquid, the reuse n-butyl alcohol is saturated is washed to neutrality, discards water liquid, and n-butyl alcohol liquid is put evaporate to dryness in the evaporating dish, residue adds methanol 1ml makes dissolving, as need testing solution.Other gets ginsenoside Rg1's reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography, draw need testing solution 10 μ l, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, lower floor's solution of placing below 10 ℃ with chloroform-methanol-water of 65:35:10 is developing solvent, launches, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color, see accompanying drawing 1;
2) get Solenognathus Gecko oral liquid 40ml, use hcl acidifying, pH value 3~4 adds the ethyl acetate jolting and extracts 3 times, each 20ml, and combined ethyl acetate liquid is put evaporate to dryness in the evaporating dish, and residue adds methanol 1ml makes dissolving, as need testing solution.Other gets the baicalin reference substance, adds methanol and makes the solution that every 1ml contains 2mg, in contrast product solution.According to thin layer chromatography test, draw need testing solution 10 μ l, reference substance solution 5 μ l put respectively on same silica gel g thin-layer plate, are developing solvent with butyl acetate-formic acid-water of 1:1:1, launch, and take out, and dry, and spray is with 3% ferric chloride alcoholic solution.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color, see accompanying drawing 2;
3) get Solenognathus Gecko oral liquid 60ml, add the ethyl acetate jolting and extract 3 times, each 40ml, combined ethyl acetate liquid is put evaporate to dryness in the evaporating dish, and residue adds ethyl acetate 0.5ml makes dissolving, as need testing solution.Other gets the Hesperidin reference substance, adds methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution.According to the thin layer chromatography test, draw need testing solution 15 μ l, reference substance solution 10 μ l, put respectively on the same silica gel g thin-layer plate that contains 0.5% sodium hydroxide, ethyl acetate-methanol-water with 100:17:13 is developing solvent, launches 5cm, and the upper solution with toluene-ethyl acetate-formic acid-water of 20:10:1:1 is developing solvent again, launch 13cm, take out, dry, spray is with the aluminum chloride test solution, put under the ultra-violet lamp and inspect, wavelength is 365nm.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color, see accompanying drawing 3;
4) get Solenognathus Gecko oral liquid 60ml, add water saturated n-butyl alcohol jolting and extract 3 times, each 30ml, merge n-butyl alcohol liquid, add 1% sodium hydroxide solution jolting and extract 3 times, each 20ml discards sodium hydroxide solution, n-butanol layer adds the saturated water washing of n-butyl alcohol 3 times, each 20ml discards water liquid, and n-butyl alcohol liquid is put evaporate to dryness in the evaporating dish, residue adds methanol 0.5ml makes dissolving, as need testing solution.Other gets the astragaloside reference substance, adds methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution.Test according to thin layer chromatography, draw need testing solution 10 μ l, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, lower floor's solution of placing below 10 ℃ with chloroform-ethyl acetate-methanol-water of 10:20:11:5 is developing solvent, launches, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color, see accompanying drawing 4;
5) check: pH value is 4.0~5.0, and the relative density Sugarless type should be not less than 1.01; Low-sugar type should be not less than 1.05; Other should meet relevant every regulation under an appendix I of mixture Chinese Pharmacopoeia version in 2010 the J item;
6) assay: according to high effective liquid chromatography for measuring;
Icariin: according to a record of Chinese Pharmacopoeia version in 2005 VI D high effective liquid chromatography for measuring.
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Acetonitrile-water with 25:75 is a mobile phase; The detection wavelength is 270nm, and column temperature is a room temperature.Number of theoretical plate calculates by the icariin peak should be not less than 1500;
The preparation of reference substance solution: it is an amount of that precision takes by weighing the icariin reference substance, uses dissolve with methanol, and be diluted to scale with methanol, shakes up, that is, the every 1ml of icariin contains 8 μ g;
The preparation of need testing solution: precision is measured Solenognathus Gecko oral liquid 40ml, and the jolting that adds diethyl ether is extracted 3 times, each 40ml, discard ether solution, water layer adds the water-saturated n-butanol jolting and extracts 4 times, and each 40ml merges n-butyl alcohol liquid, adding the jolting of 0.5mol/L sodium carbonate liquor extracts 3 times, each 40ml discards sodium carbonate liquor, evaporate to dryness in the n-butyl alcohol stratification evaporating dish, residue adds methanol 25ml makes dissolving, as need testing solution;
Algoscopy: accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, calculate, promptly.
The every 1ml of Solenognathus Gecko oral liquid contains Herba Epimedii with icariin (C 33H 40O 15) meter, must not be less than 1.35 μ g.
The high-performance liquid chromatogram determination icariin contains mensuration standard and determines explanation:
One, instrument, reagent and reagent: instrument: high performance liquid chromatograph (TSP, the U.S.); The UV100 UV-detector; Reagent: the icariin reference substance is purchased in Nat'l Pharmaceutical ﹠ Biological Products Control Institute, lot number: 110737-200413; Specification: use for assay.Reagent: acetonitrile is a chromatographically pure; Water is double distilled water.
Two, the preparation of reference substance solution: it is an amount of that precision takes by weighing the icariin reference substance, uses dissolve with methanol, and be diluted to scale with methanol, shakes up, that is, the every 1ml of icariin contains 8 μ g;
Three, the preparation of need testing solution and mensuration: precision is measured Solenognathus Gecko oral liquid 40ml, and the jolting that adds diethyl ether is extracted 3 times, each 40ml, discard ether solution, water layer adds the water-saturated n-butanol jolting and extracts 4 times, and each 40ml merges n-butyl alcohol liquid, adding the jolting of 0.5mol/L sodium carbonate liquor extracts 3 times, each 40ml discards sodium carbonate liquor, evaporate to dryness in the n-butyl alcohol stratification evaporating dish, residue adds methanol 25ml makes dissolving, as need testing solution;
Four, determining of maximum absorption wavelength: the maximum absorption wavelength that records icariin standard substance (methanol constant volume) with 762 type ultraviolet spectrophotometers is 269nm, close with the wavelength of assay under 2010 editions epimedium herb items of Chinese Pharmacopoeia, therefore determine that detecting wavelength is 270nm, sees accompanying drawing 5.
Five, mobile phase is selected: acetonitrile-water (25:75) is as this preparation Herba Epimedii assay mobile phase.
Six, chromatographic condition: with octadecylsilane chemically bonded silica is filler; With acetonitrile-water (25:75) is mobile phase; The detection wavelength is 270nm; 40 ℃ of column temperatures; Flow velocity 1ml/min.Seven, the calculating of number of theoretical plate: measure according to aforementioned chromatographic condition, measurement result is counted with the icariin peak: N=5.54 * (46.3/1.4) 2=6046, so determine to be no less than 1500 with icariin peak theory of computation plate number.
Eight, methodological study
1, the preparation of standard curve
It is an amount of that precision takes by weighing the icariin reference substance, add methanol and make the reference substance solution that every 1ml contains 37.00,18.50,9.25,4.63,2.31,1.16 μ g respectively, draw 20 μ l respectively, inject chromatograph of liquid, measure by above-mentioned chromatographic condition, with the peak area score value is vertical coordinate, icariin concentration is abscissa, the drawing standard curve gets a straight line, regression equation Y=74988x+22920, r=1.0, the result shows that icariin has good linear relationship in 0.0232 μ g~0.74 μ g scope, see accompanying drawing 6.
2, blank assay
According to prescription ratio and Solenognathus Gecko oral liquid preparation technology, make the blank sample that does not contain Herba Epimedii, make blank solution by the preparation method of test liquid again, measure in accordance with the law, the result shows that blank is noiseless to sample determination, sees accompanying drawing 7,8,9.
3, precision test
3.1 replica test
To same test sample replication 6 times, calculate relative standard deviation, icariin RSD is 1.73% as a result.Show that this method repeatability is good, the results are shown in Table 1.
Figure 198773DEST_PATH_IMAGE001
3.2 repeatability test
Different experiments personnel, different experiments chamber, different experiments instrument to same test sample replication 6 times, calculate relative standard deviation, and icariin RSD is 2.84% as a result.Show that this method repeatability is good, the results are shown in Table 2.
Figure 53596DEST_PATH_IMAGE002
4, stability test
Get same need testing solution, measure at 0,2,4,6,8,10,12 hour sample introduction respectively, results sample is stable in 12 hours, and icariin relative standard deviation RSD is 2.27%.Show that this method has good stability, and the results are shown in Table 3.
Figure 833333DEST_PATH_IMAGE003
5, recovery test
System adopts the application of sample recovery test, gets the sample 20ml that predicts content, and accurate the title decides, the accurate icariin reference substance that adds is an amount of, extracts, measures according to the test sample preparation method, calculates, the icariin average recovery rate is 99.07% as a result, n=6, RSD=2.31%.Show that this law method is accurate, the results are shown in Table 4.
÷ B * 100% A: the contained tested component content B of sample: add pure product amount C: measured value of the response rate=(C-A)
Figure 415493DEST_PATH_IMAGE004
Nine, sample determination
1, five batch sample assays
5 batch samples are measured in accordance with the law, be the results are shown in Table 5.According to measurement result, icariin content is that every ml is not less than 1.35 μ g in the tentative preparation.Limit is formulated foundation: 5 batches of average contents are 2.25 μ g/ml, float downward 40%, i.e. 1.35 μ g/ml.
Figure 167549DEST_PATH_IMAGE005
2, the medical material rate of transform
2.1 " 2005 editions epimedium herb assay methods of Chinese pharmacopoeia
Icariin is measured according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D).
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Acetonitrile-water (25:75) is a mobile phase; The detection wavelength is 270nm.Number of theoretical plate calculates by the icariin peak should be not less than 1500.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the icariin reference substance, adds methanol and make the solution that every 1ml contains 45 μ g, promptly.
The preparation of need testing solution: get Herba Epimedii blade medicinal powder (crossing sieve No. three) 0.2g, the accurate title, decide, and puts in the tool plug conical flask, the accurate Diluted Alcohol 20ml that adds, claim to decide weight, supersound process 1 hour claims to decide weight again, supplies the weight that subtracts mistake with Diluted Alcohol, shake up, filter, get subsequent filtrate, promptly.
Algoscopy: accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.
Solenognathus Gecko oral liquid blade is pressed dry product and is calculated, and contains icariin (C 33H 40O 15) meter, must not be less than 0.50%, the results are shown in Table 6.
2.2 epimedium herb preparation content determining method
Icariin: measure according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D).
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Acetonitrile-water (25:75) is a mobile phase; The detection wavelength is 270nm.Number of theoretical plate calculates by the icariin peak should be not less than 1500.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the icariin reference substance, adds methanol and make the solution that every 1ml contains 0.18mg, promptly.
The preparation of need testing solution: get Herba Epimedii blade medicinal powder (crossing sieve No. three) 1.0g, the accurate title, decide, according to preparation process with the medical material decocting in water after, filter, the filtrate jolting that adds diethyl ether is extracted 3 times, each 40ml discards ether solution, and water layer adds the water-saturated n-butanol jolting and extracts 4 times, each 40ml, merge n-butyl alcohol liquid, add the jolting of 0.5mol/L sodium carbonate liquor and extract 3 times, each 40ml, discard sodium carbonate liquor, evaporate to dryness in the n-butyl alcohol stratification evaporating dish, residue add methanol 25ml makes dissolving, as need testing solution.
Algoscopy: accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, that is, the results are shown in Table 7.
Figure 883143DEST_PATH_IMAGE007
2.3 the medical material rate of transform
Because Solenognathus Gecko oral liquid is an oral liquid, be not suitable for measuring medical material content, therefore measure, calculate its rate of transform average out to 55.02% then with the method for preparation with official method, three batches of lot numbers of three batches of corresponding respectively preparations of medical material are 0603001,0603002,0603003, the results are shown in Table 8.
Figure 82043DEST_PATH_IMAGE008

Claims (2)

1. the quality control detection method of a Solenognathus Gecko oral liquid, with Solenognathus 39.1g, Gecko 0.73g, Radix Ginseng 4.68g, Testis Et penis Caprae seu Ovis 4.68g, Testis Caprae seu Ovis 4.68g, Radix Scutellariae 4.68g, Radix Rehmanniae Preparata 3.1g, Semen Cuscutae 3.1g, Radix Polygoni Multiflori 3.1g, Radix Rehmanniae 3.1g, Pericarpium Citri Reticulatae 3.1g, Radix Angelicae Sinensis 1.56g, Radix Astragali 4.68g, Actinolitum 1.56g, Stamen Nelumbinis 1.56g, Radix Glycyrrhizae 1.56g, Rhizoma Chuanxiong 1.56g, Rhizoma Alismatis 1.56g, Herba Cynomorii 1.56g, Fructus Amomi Rotundus 1.56g, Lignum Aquilariae Resinatum 1.56g, Cornu Cervi Pantotrichum 1.56g, Fructus Lycii 1.56g, Herba Cistanches 0.78g, Adeps Caprae seu ovis Herba Epimedii Preparata 1.56g, Cortex Cinnamomi 1.56g, Semen Allii Tuberosi 1.56g, Fructus Cnidii 1.56g, Pericarpium Zanthoxyli 0.31g decocts with water secondary, each 2 hours, collecting decoction, being concentrated into relative density at 80 ℃ is 1.04~1.06 clear paste, add the ethanol qdx, cold preservation 12 hours, filter, concentrate, add water, cold preservation, filter, filtrate adds benzoic acid makes dissolving in right amount, with 8% sodium hydroxide adjust pH 4.6~4.8, add correctives xylitol 3%, adjust total amount to 1000ml, filter, packing, sterilization, that is, its feature may further comprise the steps:
1) get Solenognathus Gecko oral liquid 30ml, the 20ml that adds diethyl ether, jolting is extracted, place, discard ether solution, water layer is with water saturated n-butanol extraction 3 times, consumption is followed successively by 20ml, 15ml, 15ml, merges n-butyl alcohol liquid, adds 4% potassium hydroxide solution 30ml washing once, discard washing liquid, the reuse n-butyl alcohol is saturated is washed to neutrality, discards water liquid, and n-butyl alcohol liquid is put evaporate to dryness in the evaporating dish, residue adds methanol 1ml makes dissolving, as need testing solution; Other gets ginsenoside Rg1's reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution;
Test according to thin layer chromatography, draw need testing solution 10 μ l, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, lower floor's solution of placing below 10 ℃ with chloroform-methanol-water of 65:35:10 is developing solvent, launches, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
2) get Solenognathus Gecko oral liquid 40ml, use hcl acidifying, pH value 3~4 adds the ethyl acetate jolting and extracts 3 times, each 20ml, and combined ethyl acetate liquid is put evaporate to dryness in the evaporating dish, and residue adds methanol 1ml makes dissolving, as need testing solution; Other gets the baicalin reference substance, adds methanol and makes the solution that every 1ml contains 2mg, in contrast product solution; According to thin layer chromatography test, draw need testing solution 10 μ l, reference substance solution 5 μ l put respectively on same silica gel g thin-layer plate, are developing solvent with butyl acetate-formic acid-water of 1:1:1, launch, and take out, and dry, and spray is with 3% ferric chloride alcoholic solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
3) get Solenognathus Gecko oral liquid 60ml, add the ethyl acetate jolting and extract 3 times, each 40ml, combined ethyl acetate liquid is put evaporate to dryness in the evaporating dish, and residue adds ethyl acetate 0.5ml makes dissolving, as need testing solution; Other gets the Hesperidin reference substance, adds methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution; According to the thin layer chromatography test, draw need testing solution 15 μ l, reference substance solution 10 μ l, put respectively on the same silica gel g thin-layer plate that contains 0.5% sodium hydroxide, ethyl acetate-methanol-water with 100:17:13 is developing solvent, launches 5cm, and the upper solution with toluene-ethyl acetate-formic acid-water of 20:10:1:1 is developing solvent again, launch 13cm, take out, dry, spray is with the aluminum chloride test solution, put under the ultra-violet lamp and inspect, wavelength is 365nm; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
4) get Solenognathus Gecko oral liquid 60ml, add water saturated n-butyl alcohol jolting and extract 3 times, each 30ml, merge n-butyl alcohol liquid, add 1% sodium hydroxide solution jolting and extract 3 times, each 20ml discards sodium hydroxide solution, n-butanol layer adds the saturated water washing of n-butyl alcohol 3 times, each 20ml discards water liquid, and n-butyl alcohol liquid is put evaporate to dryness in the evaporating dish, residue adds methanol 0.5ml makes dissolving, as need testing solution; Other gets the astragaloside reference substance, adds methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer chromatography, draw need testing solution 10 μ l, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, lower floor's solution of placing below 10 ℃ with chloroform-ethyl acetate-methanol-water of 10:20:11:5 is developing solvent, launches, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
5) check: pH value is 4.0~5.0, and the relative density Sugarless type is not less than 1.01, and low-sugar type is not less than 1.05; Other should meet relevant every regulation under an appendix I of mixture Chinese Pharmacopoeia version in 2010 the J item;
6) assay: icariin is according to high effective liquid chromatography for measuring;
Icariin:According to an appendix VI of Chinese Pharmacopoeia version in 2010 D high effective liquid chromatography for measuring;
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Acetonitrile-water with 25:75 is a mobile phase; The detection wavelength is 270nm, and column temperature is a room temperature; Number of theoretical plate calculates by the icariin peak should be not less than 1500;
The preparation of reference substance solution: it is an amount of that precision takes by weighing the icariin reference substance, uses dissolve with methanol, and be diluted to scale with methanol, shakes up, that is, the every 1ml of icariin contains 8 μ g;
The preparation of need testing solution:Precision is measured Solenognathus Gecko oral liquid 40ml, and the jolting that adds diethyl ether is extracted 3 times, each 40ml, discard ether solution, water layer adds the water-saturated n-butanol jolting and extracts 4 times, and each 40ml merges n-butyl alcohol liquid, adding the jolting of 0.5mol/L sodium carbonate liquor extracts 3 times, each 40ml discards sodium carbonate liquor, evaporate to dryness in the n-butyl alcohol stratification evaporating dish, residue adds methanol 25ml makes dissolving, as need testing solution;
Algoscopy: accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, calculate, promptly.
2. the quality control detection method of a kind of Solenognathus Gecko oral liquid according to claim 1 is characterized in that it is C with the icariin molecular formula that the every 1ml of Solenognathus Gecko oral liquid contains Herba Epimedii 33H 40O 15Meter must not be less than 1.35 μ g.
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CN106198834A (en) * 2016-06-24 2016-12-07 广西灵峰药业有限公司 The quality of production control method of juice mended by the one seed ginseng stilbene Radix Polygoni Multiflori
CN107737191A (en) * 2017-09-22 2018-02-27 内蒙古蒙肽生物工程有限公司 The saline cistanche composition and preparation technology of a kind of kidney-tonifying health-care
CN112083097A (en) * 2020-09-09 2020-12-15 四川新绿色药业科技发展有限公司 Thin-layer identification method for simultaneously identifying ferulic acid, calycosin glucoside and hesperidin
CN114113381A (en) * 2021-11-12 2022-03-01 山东省食品药品检验研究院 Characteristic polypeptide of saloon, application thereof and method for identifying comfortable saloon
CN115400077A (en) * 2022-09-22 2022-11-29 山东宏济堂制药集团股份有限公司 Application of sea dragon and gecko oral liquid in preparation of medicine for treating allergic rhinitis
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CN107737191A (en) * 2017-09-22 2018-02-27 内蒙古蒙肽生物工程有限公司 The saline cistanche composition and preparation technology of a kind of kidney-tonifying health-care
CN112083097A (en) * 2020-09-09 2020-12-15 四川新绿色药业科技发展有限公司 Thin-layer identification method for simultaneously identifying ferulic acid, calycosin glucoside and hesperidin
CN114113381A (en) * 2021-11-12 2022-03-01 山东省食品药品检验研究院 Characteristic polypeptide of saloon, application thereof and method for identifying comfortable saloon
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CN115475219A (en) * 2022-09-22 2022-12-16 山东宏济堂制药集团股份有限公司 Application of sea dragon and gecko oral liquid in preparation of medicine for treating senile dementia
CN115400077B (en) * 2022-09-22 2024-01-26 山东宏济堂制药集团股份有限公司 Application of sea dragon gecko oral liquid in preparation of medicines for treating allergic rhinitis
CN115475219B (en) * 2022-09-22 2024-01-26 山东宏济堂制药集团股份有限公司 Application of sea dragon gecko oral liquid in preparation of medicine for treating senile dementia

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