CN107621517B - Detection method of kechuanjing syrup - Google Patents
Detection method of kechuanjing syrup Download PDFInfo
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Abstract
The invention relates to a detection method of cough and asthma syrup for a traditional Chinese medicine compound preparation prepared from traditional Chinese medicinal materials of platycodon grandiflorum, aster tataricus, earthworm, rhizoma anemarrhenae, dandelion, scutellaria baicalensis, trichosanthes kirilowii maxim, ophiopogon japonicus, bitter apricot seed, coltsfoot flower, honey radix stemonae, liquorice, red paeony root and salvia miltiorrhiza. The method can effectively control the quality of the kechuanjing syrup, and can be used as a method for controlling the quality of the medicine and observing the process reliability.
Description
Technical Field
The invention relates to a detection method of a medicine for treating chronic bronchitis, bronchial asthma, acute pharyngitis, infantile pneumonia and other symptoms, belonging to the field of pharmacy.
Background
The kechuanjing syrup is prepared according to the standard issued by the ministry of medicine, has the functions of relieving cough and asthma, eliminating phlegm and diminishing inflammation, and is used for treating chronic bronchitis, bronchial asthma, acute pharyngitis, infantile pneumonia and other diseases. The medicine is prepared from traditional Chinese medicinal materials of platycodon grandiflorum, aster tataricus, earthworm, rhizoma anemarrhenae, dandelion, scutellaria baicalensis, trichosanthes kirilowii maxim, radix ophiopogonis, bitter almond, tussilago, honey stemona, liquorice, red paeony root and salvia miltiorrhiza; wherein, the scutellaria, the ophiopogon root and the like are the medicinal materials with the main treatment function. In the existing execution standard quality control method of the kechuanjing syrup, a quality control method for the medicinal materials with main treatment effects is lacked; therefore, the prior art has limitation in comprehensively evaluating the quality of the kechuanjing syrup. The invention overcomes the defects of the prior art, improves the quality control standard of the kechuanjing syrup, increases the quality control method for measuring the content of baicalin (baicalin) and the qualitative identification method for thin-layer chromatography of baicalin, paeoniflorin, sarsasapogenin, sodium danshensu and Chinese medicinal material radix ophiopogonis, and further improves the quality control standard of the compound preparation.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, improve and establish a quality control method of the kechuanjing syrup, add a quality control method for measuring the content of baicalin (baicalin) and a thin-layer chromatography qualitative identification method for baicalin, paeoniflorin, sarsasapogenin, sodium danshensu and traditional Chinese medicinal materials ophiopogon root, and further improve the quality control standard of the compound preparation; can effectively control the product quality of the cough and asthma relieving syrup.
The invention is realized by the following technical scheme:
1, the content of baicalin contained in the traditional Chinese medicine scutellaria baicalensis of the kechuanjing syrup is determined by a high performance liquid chromatography:
a. chromatographic conditions and system applicability test, octadecylsilane chemically bonded silica is used as a filler, and methanol-water-phosphoric acid 47: 53: 0.2 is mobile phase; the detection wavelength is 280nm, and the number of theoretical plates is not less than 3000 calculated according to baicalin peak;
b. preparing a reference solution, namely precisely weighing a proper amount of a baicalin reference substance, and adding diluted ethanol to prepare a solution containing 25-35 mug of baicalin per 1ml serving as the reference solution;
c. preparing a test solution by precisely measuring 8-12 ml of kechuanjing syrup, placing in a 100ml measuring flask, dissolving with water and diluting to scale, shaking, precisely measuring 5ml, placing in a 50ml measuring flask, dissolving with diluted ethanol and diluting to scale, shaking, filtering, and collecting the filtrate as the test solution;
d. the determination method comprises precisely sucking 8-12 μ l of reference solution and sample solution respectively, injecting into liquid chromatograph, and determining;
2, identifying the baicalin in the kechuanjing syrup by using a thin-layer chromatography:
a. preparing reference solution by adding methanol into baicalin reference to obtain 1mg solution per 1ml as reference solution;
b. preparing test solution by collecting kechuanjing syrup 8ml-12ml, adding water 10ml, shaking, placing on D101 type macroporous adsorbent resin column with inner diameter of 1.5cm and height of 12cm, eluting with water 80ml, discarding water washing solution, eluting with 40% ethanol 60ml, collecting eluate, evaporating to dryness, adding methanol 3ml into residue, slightly heating and stirring for dissolving, centrifuging, and collecting supernatant as test solution;
c. the thin layer chromatography test comprises respectively dropping 3-8 μ l of the above reference solution and test solution on the same silica gel G thin layer plate, developing with ethyl acetate-butanone-formic acid-water 5:3:1:1 as developing agent, taking out, air drying, spraying 1% ferric trichloride ethanol solution, and displaying spots of the same color in the test solution chromatogram at the position corresponding to the reference solution chromatogram;
3, identifying paeoniflorin in the kechuanjing syrup by using a thin-layer chromatography:
a. preparing control solution by adding methanol into penoniflorin control drug to obtain 1mg solution per 1ml as control solution;
b. preparing test solution by collecting kechuanjing syrup 8ml-12ml, adding water 10ml, shaking, placing on D101 type macroporous adsorbent resin column with inner diameter of 1.5cm and height of 12cm, eluting with water 80ml, discarding water washing solution, eluting with 40% ethanol 60ml, collecting eluate, evaporating to dryness, adding methanol 3ml into residue, slightly heating and stirring for dissolving, centrifuging, and collecting supernatant as test solution;
c. performing thin layer chromatography test, namely sucking 3-8 μ l of each of the reference solution and the test solution, respectively dropping on the same silica gel G thin layer plate, developing with chloroform-methanol-water 9:3:0.3 as developing agent, taking out, air drying, spraying with 5% vanillin-sulfuric acid solution, heating at 105 deg.C until the spots are clearly developed, and displaying spots with the same color in the chromatogram of the test solution at the position corresponding to the chromatogram of the reference solution;
4, identifying the sarsasapogenin in the syrup for treating cough and asthma by using a thin-layer chromatography:
a. the reference solution is prepared by adding methanol into sarsasapogenin reference to obtain 1mg solution per 1ml as reference solution;
b. preparing test solution by collecting kechuanjing syrup 8ml-12ml, adding water 10ml, shaking, placing on D101 type macroporous adsorbent resin column with inner diameter of 1.5cm and height of 12cm, eluting with water 80ml, discarding water washing solution, eluting with 40% ethanol 60ml, collecting eluate, evaporating to dryness, adding methanol 3ml into residue, stirring slightly to dissolve, centrifuging, collecting supernatant, placing on D101 type macroporous adsorbent resin column, eluting with 70% ethanol 60ml, collecting eluate, adding hydrochloric acid 1-3ml, heating and refluxing for 1 hr, concentrating to 1-3ml, adding water 15-25ml to dissolve, shaking and extracting with ethyl acetate for 2 times, each time 20-40ml, mixing ethyl acetate solutions, evaporating to dryness, adding methanol 1-3ml into residue to dissolve, and using as test solution;
c. taking 5-10 μ l of each of the reference solution and the sample solution, respectively dropping on the same silica gel G thin layer plate, developing with toluene-acetone 9:1 as developing agent, taking out, air drying, spraying 5% vanillin sulfuric acid solution, heating at 105 deg.C until the spots are clearly developed, and displaying spots with the same color in the sample chromatogram at the position corresponding to the reference chromatogram;
5, identifying sodium danshensu in the syrup for treating cough and asthma by using a thin-layer chromatography:
a. preparing reference solution by adding 75% methanol into sodium danshensu reference solution to obtain 1mg solution per 1ml as reference solution;
b. preparing test solution by collecting kechuanjing syrup 10-20ml, adding water 10-20ml, shaking, adjusting pH to 2 with dilute hydrochloric acid, extracting with ethyl acetate under shaking for 2 times (20-40 ml each time), mixing ethyl acetate solutions, evaporating to dryness, and dissolving the residue with methanol 1-3ml to obtain test solution;
c. thin layer chromatography test comprises respectively dropping 2-5 μ l of the above reference solution and sample solution on the same silica gel G thin layer plate, developing with toluene-ethyl acetate-formic acid 5:5:1 as developing agent, taking out, air drying, fumigating in ammonia vapor, and inspecting with ultraviolet lamp at 365nm to obtain spots of the same color in the sample chromatogram at the position corresponding to the reference chromatogram;
the thin-layer chromatography identification of the 6 kechuanjing syrup traditional Chinese medicine radix ophiopogonis:
a. preparing control solution by decocting radix Ophiopogonis 1g with water 25-35ml for 30 min, cooling, filtering, and collecting filtrate as control solution;
b. the test solution is prepared by collecting kechuanjing syrup 5-15ml, adding water 15-25ml, shaking, adding hydrochloric acid 1-3ml, heating and refluxing for 1 hr, cooling, extracting with diethyl ether 20-40ml, volatilizing diethyl ether solution, and dissolving the residue with chloroform 1-3ml to obtain test solution;
c. and (3) performing thin-layer chromatography test, namely sucking the reference medicinal material solution and the test sample solution by 2-5 mu l respectively, dropping the reference medicinal material solution and the test sample solution on the same silica gel G thin-layer plate, developing by taking trichloromethane-acetone 4:1 as a developing agent, taking out, drying in the air, spraying 10% sulfuric acid ethanol solution, heating at 105 ℃ for 5 minutes, and displaying spots with the same color on the positions corresponding to the reference medicinal material chromatogram in the test sample chromatogram.
The invention provides a quality control method for measuring the content of baicalin and a thin-layer chromatography qualitative identification method for baicalin, paeoniflorin, smilagenin, sodium danshensu and Chinese medicinal material dwarf lilyturf tuber, the method is simple and easy to implement, and can be used as a quality control index of cough and asthma syrup.
Detailed Description
Example (b):
taking 100g of platycodon grandiflorum, 100g of aster tataricus, 120g of earthworm, 150g of rhizoma anemarrhenae, 150g of dandelion, 150g of scutellaria baicalensis, 200g of trichosanthes kirilowii maxim, 100g of radix ophiopogonis, 100g of bitter apricot seed, 100g of tussilago farfara, 100g of honey stemona, 100g of liquorice, 120g of radix paeoniae rubra and 120g of salvia miltiorrhiza in the formula, adding water, decocting for 2 times, decocting for 2 hours for the first time and 1 hour for the second time, combining decoctions, filtering, concentrating the filtrate to 2000ml, standing for 24 hours, pouring out supernatant, concentrating to a proper amount, adding 660g of sucrose, stirring uniformly to dissolve, adding 3g of sodium benzoate and water to 1200ml, standing for 48 hours, adding.
The quality control method of the kechuanjing syrup comprises the following steps:
1, the content of baicalin contained in the traditional Chinese medicine scutellaria baicalensis of the kechuanjing syrup is determined by a high performance liquid chromatography:
a. chromatographic conditions and system applicability test, octadecylsilane chemically bonded silica is used as a filler, and methanol-water-phosphoric acid 47: 53: 0.2 is mobile phase; the detection wavelength is 280nm, and the number of theoretical plates is not less than 3000 calculated according to baicalin peak;
b. preparing a reference solution, namely precisely weighing a proper amount of baicalin reference, and adding diluted ethanol to prepare a solution containing 30 microgram of baicalin per 1ml as the reference solution;
c. preparing a test solution by precisely measuring 10ml of kechuanjing syrup, placing in a 100ml measuring flask, dissolving with water and diluting to scale, shaking, precisely measuring 5ml, placing in a 50ml measuring flask, dissolving with diluted ethanol and diluting to scale, shaking, filtering, and collecting the filtrate as the test solution;
d. the determination method comprises precisely sucking 10 μ l of reference solution and test solution respectively, injecting into liquid chromatograph, and determining; the content of Scutellariae radix in per 1ml of KECHUANJING syrup is not less than 1.5mg (calculated as baicalin);
2, identifying the baicalin in the kechuanjing syrup by using a thin-layer chromatography:
a. preparing reference solution by adding methanol into baicalin reference to obtain 1mg solution per 1ml as reference solution;
b. preparing test solution by collecting 10ml of KECHUANJING syrup, adding 10ml of water, shaking, placing on D101 type macroporous adsorbent resin column with inner diameter of 1.5cm and height of 12cm, eluting with 80ml of water, discarding water washing solution, eluting with 60ml of 40% ethanol, collecting eluate, evaporating to dry, adding 3ml of methanol into residue, slightly heating, stirring for dissolving, centrifuging, and collecting supernatant as test solution;
c. the thin layer chromatography test comprises respectively dropping 3-8 μ l of the above reference solution and test solution on the same silica gel G thin layer plate, developing with ethyl acetate-butanone-formic acid-water 5:3:1:1 as developing agent, taking out, air drying, spraying 1% ferric trichloride ethanol solution, and displaying spots of the same color in the test solution chromatogram at the position corresponding to the reference solution chromatogram;
3, identifying paeoniflorin in the kechuanjing syrup by using a thin-layer chromatography:
a. preparing control solution by adding methanol into penoniflorin control drug to obtain 1mg solution per 1ml as control solution;
b. preparing test solution by collecting 10ml of KECHUANJING syrup, adding 10ml of water, shaking, placing on D101 type macroporous adsorbent resin column with inner diameter of 1.5cm and height of 12cm, eluting with 80ml of water, discarding water washing solution, eluting with 60ml of 40% ethanol, collecting eluate, evaporating to dry, adding 3ml of methanol into residue, slightly heating, stirring for dissolving, centrifuging, and collecting supernatant as test solution;
c. performing thin layer chromatography test, namely sucking 3-8 μ l of each of the reference solution and the test solution, respectively dropping on the same silica gel G thin layer plate, developing with chloroform-methanol-water 9:3:0.3 as developing agent, taking out, air drying, spraying with 5% vanillin-sulfuric acid solution, heating at 105 deg.C until the spots are clearly developed, and displaying spots with the same color in the chromatogram of the test solution at the position corresponding to the chromatogram of the reference solution;
4, identifying the sarsasapogenin in the syrup for treating cough and asthma by using a thin-layer chromatography:
a. the reference solution is prepared by adding methanol into sarsasapogenin reference to obtain 1mg solution per 1ml as reference solution;
b. preparing test solution by collecting 10ml of KECHUANJING syrup, adding 10ml of water, shaking, placing on D101 type macroporous adsorbent resin column with inner diameter of 1.5cm and height of 12cm, eluting with 80ml of water, discarding water washing solution, eluting with 60ml of 40% ethanol, collecting eluate, evaporating to dry, adding 3ml of methanol into residue, slightly heating and stirring for dissolving, centrifuging, collecting supernatant, placing on D101 type macroporous adsorbent resin column, eluting with 60ml of 70% ethanol, collecting eluate, adding 2ml of hydrochloric acid, heating and refluxing for 1 hr, concentrating to 2ml, adding 20ml of water for dissolving, shaking and extracting with ethyl acetate for 2 times, 30ml each time, mixing ethyl acetate solutions, evaporating to dry, adding 2ml of methanol into residue for dissolving to obtain test solution;
c. taking 5-10 μ l of each of the reference solution and the sample solution, respectively dropping on the same silica gel G thin layer plate, developing with toluene-acetone 9:1 as developing agent, taking out, air drying, spraying 5% vanillin sulfuric acid solution, heating at 105 deg.C until the spots are clearly developed, and displaying spots with the same color in the sample chromatogram at the position corresponding to the reference chromatogram;
5, identifying sodium danshensu in the syrup for treating cough and asthma by using a thin-layer chromatography:
a. preparing reference solution by adding 75% methanol into sodium danshensu reference solution to obtain 1mg solution per 1ml as reference solution;
b. the test solution is prepared by collecting kechuanjing syrup 15ml, adding water 15ml, shaking, adjusting pH to 2 with dilute hydrochloric acid, extracting with ethyl acetate under shaking for 2 times (30 ml each time), mixing ethyl acetate solutions, evaporating to dryness, and dissolving the residue with methanol 2ml to obtain test solution;
c. thin layer chromatography test comprises respectively dropping 2-5 μ l of the above reference solution and sample solution on the same silica gel G thin layer plate, developing with toluene-ethyl acetate-formic acid 5:5:1 as developing agent, taking out, air drying, fumigating in ammonia vapor, and inspecting with ultraviolet lamp at 365nm to obtain spots of the same color in the sample chromatogram at the position corresponding to the reference chromatogram;
the thin-layer chromatography identification of the 6 kechuanjing syrup traditional Chinese medicine radix ophiopogonis:
a. the control solution is prepared by decocting radix Ophiopogonis 1g with water 30ml for 30 min, cooling, filtering, and collecting filtrate as control solution;
b. the test solution is prepared by collecting kechuanjing syrup 10ml, adding water 20ml, shaking, adding hydrochloric acid 2ml, heating and refluxing for 1 hr, cooling, extracting with diethyl ether 30ml, volatilizing diethyl ether solution, and dissolving the residue with chloroform 2ml to obtain test solution;
c. and (3) performing thin-layer chromatography test, namely sucking the reference medicinal material solution and the test sample solution by 2-5 mu l respectively, dropping the reference medicinal material solution and the test sample solution on the same silica gel G thin-layer plate, developing by taking trichloromethane-acetone 4:1 as a developing agent, taking out, drying in the air, spraying 10% sulfuric acid ethanol solution, heating at 105 ℃ for 5 minutes, and displaying spots with the same color on the positions corresponding to the reference medicinal material chromatogram in the test sample chromatogram.
Claims (1)
1. A detection method of cough and asthma relieving syrup is disclosed, wherein the cough and asthma relieving syrup is prepared from 100g of platycodon grandiflorum, 100g of aster, 120g of earthworm, 150g of rhizoma anemarrhenae, 150g of dandelion, 150g of scutellaria baicalensis, 200g of trichosanthes kirilowii maxim, 100g of radix ophiopogonis, 100g of bitter apricot kernel, 100g of common coltsfoot flower, 100g of honey radix stemonae, 100g of liquorice, 120g of red paeony root and 120g of salvia miltiorrhiza, and is characterized by comprising the following steps:
(1) the content of baicalin contained in the traditional Chinese medicine scutellaria baicalensis of the kechuanjing syrup is determined by a high performance liquid chromatography:
a. chromatographic conditions and system applicability test, octadecylsilane chemically bonded silica is used as a filler, and methanol-water-phosphoric acid 47: 53: 0.2 is mobile phase; the detection wavelength is 280nm, and the number of theoretical plates is not less than 3000 calculated according to baicalin peak;
b. preparing a reference solution, namely precisely weighing a proper amount of a baicalin reference substance, and adding diluted ethanol to prepare a solution containing 25-35 mug of baicalin per 1ml serving as the reference solution;
c. preparing a test solution by precisely measuring 8-12 ml of kechuanjing syrup, placing in a 100ml measuring flask, dissolving with water and diluting to scale, shaking, precisely measuring 5ml, placing in a 50ml measuring flask, dissolving with diluted ethanol and diluting to scale, shaking, filtering, and collecting the filtrate as the test solution;
d. the determination method comprises precisely sucking 8-12 μ l of reference solution and sample solution respectively, injecting into liquid chromatograph, and determining;
(2) the baicalin in the kechuanjing syrup is identified by a thin-layer chromatography:
a. preparing reference solution by adding methanol into baicalin reference to obtain 1mg solution per 1ml as reference solution;
b. preparing test solution by collecting kechuanjing syrup 8ml-12ml, adding water 10ml, shaking, placing on D101 type macroporous adsorbent resin column with inner diameter of 1.5cm and height of 12cm, eluting with water 80ml, discarding water washing solution, eluting with 40% ethanol 60ml, collecting eluate, evaporating to dryness, adding methanol 3ml into residue, slightly heating and stirring for dissolving, centrifuging, and collecting supernatant as test solution;
c. the thin layer chromatography test comprises respectively dropping 3-8 μ l of the above reference solution and test solution on the same silica gel G thin layer plate, developing with ethyl acetate-butanone-formic acid-water 5:3:1:1 as developing agent, taking out, air drying, spraying 1% ferric trichloride ethanol solution, and displaying spots of the same color in the test solution chromatogram at the position corresponding to the reference solution chromatogram;
(3) the paeoniflorin in the kechuanjing syrup is identified by a thin-layer chromatography:
a. preparing control solution by adding methanol into penoniflorin control drug to obtain 1mg solution per 1ml as control solution;
b. preparing test solution by collecting kechuanjing syrup 8ml-12ml, adding water 10ml, shaking, placing on D101 type macroporous adsorbent resin column with inner diameter of 1.5cm and height of 12cm, eluting with water 80ml, discarding water washing solution, eluting with 40% ethanol 60ml, collecting eluate, evaporating to dryness, adding methanol 3ml into residue, slightly heating and stirring for dissolving, centrifuging, and collecting supernatant as test solution;
c. performing thin layer chromatography test, namely sucking 3-8 μ l of each of the reference solution and the test solution, respectively dropping on the same silica gel G thin layer plate, developing with chloroform-methanol-water 9:3:0.3 as developing agent, taking out, air drying, spraying with 5% vanillin-sulfuric acid solution, heating at 105 deg.C until the spots are clearly developed, and displaying spots with the same color in the chromatogram of the test solution at the position corresponding to the chromatogram of the reference solution;
(4) the sarsasapogenin in the kechuanjing syrup is identified by a thin-layer chromatography:
a. the reference solution is prepared by adding methanol into sarsasapogenin reference to obtain 1mg solution per 1ml as reference solution;
b. preparing test solution by collecting kechuanjing syrup 8ml-12ml, adding water 10ml, shaking, placing on D101 type macroporous adsorbent resin column with inner diameter of 1.5cm and height of 12cm, eluting with water 80ml, discarding water washing solution, eluting with 40% ethanol 60ml, collecting eluate, evaporating to dryness, adding methanol 3ml into residue, stirring slightly to dissolve, centrifuging, collecting supernatant, placing on D101 type macroporous adsorbent resin column, eluting with 70% ethanol 60ml, collecting eluate, adding hydrochloric acid 1-3ml, heating and refluxing for 1 hr, concentrating to 1-3ml, adding water 15-25ml to dissolve, shaking and extracting with ethyl acetate for 2 times, each time 20-40ml, mixing ethyl acetate solutions, evaporating to dryness, adding methanol 1-3ml into residue to dissolve, and using as test solution;
c. taking 5-10 μ l of each of the reference solution and the sample solution, respectively dropping on the same silica gel G thin layer plate, developing with toluene-acetone 9:1 as developing agent, taking out, air drying, spraying 5% vanillin sulfuric acid solution, heating at 105 deg.C until the spots are clearly developed, and displaying spots with the same color in the sample chromatogram at the position corresponding to the reference chromatogram;
(5) the sodium danshensu in the syrup for treating cough and asthma is identified by thin-layer chromatography:
a. preparing reference solution by adding 75% methanol into sodium danshensu reference solution to obtain 1mg solution per 1ml as reference solution;
b. preparing test solution by collecting kechuanjing syrup 10-20ml, adding water 10-20ml, shaking, adjusting pH to 2 with dilute hydrochloric acid, extracting with ethyl acetate under shaking for 2 times (20-40 ml each time), mixing ethyl acetate solutions, evaporating to dryness, and dissolving the residue with methanol 1-3ml to obtain test solution;
c. thin layer chromatography test comprises respectively dropping 2-5 μ l of the above reference solution and sample solution on the same silica gel G thin layer plate, developing with toluene-ethyl acetate-formic acid 5:5:1 as developing agent, taking out, air drying, fumigating in ammonia vapor, and inspecting with ultraviolet lamp at 365nm to obtain spots of the same color in the sample chromatogram at the position corresponding to the reference chromatogram;
(6) the cough and asthma relieving syrup traditional Chinese medicine radix ophiopogonis is identified by a thin-layer chromatography:
a. preparing control solution by decocting radix Ophiopogonis 1g with water 25-35ml for 30 min, cooling, filtering, and collecting filtrate as control solution;
b. the test solution is prepared by collecting kechuanjing syrup 5-15ml, adding water 15-25ml, shaking, adding hydrochloric acid 1-3ml, heating and refluxing for 1 hr, cooling, extracting with diethyl ether 20-40ml, volatilizing diethyl ether solution, and dissolving the residue with chloroform 1-3ml to obtain test solution;
c. and (3) performing thin-layer chromatography test, namely sucking the reference medicinal material solution and the test sample solution by 2-5 mu l respectively, dropping the reference medicinal material solution and the test sample solution on the same silica gel G thin-layer plate, developing by taking trichloromethane-acetone 4:1 as a developing agent, taking out, drying in the air, spraying 10% sulfuric acid ethanol solution, heating at 105 ℃ for 5 minutes, and displaying spots with the same color on the positions corresponding to the reference medicinal material chromatogram in the test sample chromatogram.
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