CN109975469A - The quality determining method of dog kidney in a kind of NANBAO JIAONANG - Google Patents

The quality determining method of dog kidney in a kind of NANBAO JIAONANG Download PDF

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Publication number
CN109975469A
CN109975469A CN201711450165.9A CN201711450165A CN109975469A CN 109975469 A CN109975469 A CN 109975469A CN 201711450165 A CN201711450165 A CN 201711450165A CN 109975469 A CN109975469 A CN 109975469A
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thin
dog
nanbao jiaonang
layer chromatography
nanbao
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不公告发明人
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Suzhou Tang Kunchen Amperex Technology Ltd
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Suzhou Tang Kunchen Amperex Technology Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/90Plate chromatography, e.g. thin layer or paper chromatography

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The invention discloses a kind of quality determining methods of dog kidney in NANBAO JIAONANG, it is to take this product content 2.0g, petroleum ether 10ml is added, after ultrasonic extraction 30 minutes, centrifuging and taking supernatant is sample solution, it is measured according to thin layer chromatography, take sample solution 10ul point sample on silica gel g thin-layer plate, using volume ratio for 1:5:2:3 benzene-n-hexane-acetone and ethyl acetate mixed liquor as solvent, after 11-15cm is unfolded, it takes out, it dries, it sets respectively and observes thin-layer chromatography under ultraviolet lamp 365nm, and 5% ethanol solution of sulfuric acid of even spraying on lamellae, 100 DEG C of heating are after ten minutes, observed under daylight thin-layer chromatography is set again;If in the chromatography of above two view mode, one of multiple spots obtained in lamellae have fluorescence spot near Rf value 0.5, and have color change after spraying color developing agent, then dog renal drug material effective component exists in NANBAO JIAONANG.Method sensitivity of the invention is good, and specificity is strong, corresponding negative noiseless.Can the true and false superiority and inferiority to NANBAO JIAONANG in the market identify.

Description

The quality determining method of dog kidney in a kind of NANBAO JIAONANG
Technical field
The present invention relates to the quality determining methods of compound Chinese medicinal preparation, and in particular to a kind of traditional Chinese medicine for invigorating kidney and strengthening yang compound system The quality determining method of dog kidney in agent NANBAO JIAONANG.
Background technique
NANBAO JIAONANG is traditional Chinese medicine compound preparation.Simply by pilose antler, hippocampus, donkey kidney, dog kidney, ginseng, Radix Angelicae Sinensis etc. 30 Rare medicinal herbs composition, has the effect of strengthening yang and invigorating kidney, enriching yin qi-restoratives, strengthening the muscles and bones, can be used for the insufficiency of the kidney yang, impotence slipping diarrhea, waist Legs, the scrotum is clammy, the diseases such as apathetic, loss of appetite, and effect is obvious.However traditional Chinese medicine ingredients are more complicated, existing male Health-care capsule preparation national standard is that hygienic ministerial standard 19, Chinese medicine is recorded, and quality control index is few, and quality standard falls behind, other side Middle Radix Angelicae Sinensis has carried out Qualitive test.Dog kidney has effects that have kidney-reinforcing Yang-strengthening, strengthen muscles and bones in NANBAO JIAONANG side, can treat impotence not The diseases such as act, soreness and weakness of waist and knees, play a major role in side.At present both at home and abroad not to the report of dog kidney detection method.Therefore it examines It surveys in NANBAO JIAONANG and whether contains dog kidney, enhance the quality controllability of this product, it is imperative.
Summary of the invention
The purpose of the present invention is to provide a kind of quality determining methods of dog kidney in controllable NANBAO JIAONANG, can be effective Dog kidney in other side carries out Qualitive test, and specificity is good, favorable reproducibility, stability are strong.
The quality determining method of dog kidney in a kind of NANBAO JIAONANG, it is characterised in that:
This product content 2.0g is taken, petroleum ether 10ml is added, after ultrasonic extraction 30 minutes, centrifuging and taking supernatant is sample solution, Measured according to thin layer chromatography, take sample solution 10ul point sample on silica gel g thin-layer plate, with volume ratio for 1:5:2:3 benzene-just oneself Alkane-acetone and ethyl acetate mixed liquor is as solvent, after 11-15cm is unfolded, takes out, dries, set ultraviolet lamp 365nm respectively Lower observation thin-layer chromatography, and 5% ethanol solution of sulfuric acid of even spraying on lamellae, 100 DEG C of heating after ten minutes, then set daylight Lower observation thin-layer chromatography;If in the chromatography of above two view mode, one of multiple spots are in Rf value 0.5 obtained in lamellae Nearby there is fluorescence spot, and have color change after spraying color developing agent, then dog renal drug material effective component exists in NANBAO JIAONANG.
One of several spots obtained in the Chinese materia medica preparation sample solution are in hyacinthine near Rf value 0.5, then treasure for Man Dog renal drug material effective component exists in capsule.
The method can be used for dog renal drug in other form of Chinese drug, including pill, granule, capsule, Tabules The detection of material effective component.
The present inventor is final to obtain using dog kidney in tlc determination NANBAO JIAONANG in a large amount of experimental basis Measuring method is realized and is examined to the qualitative quality of monarch drug in a prescription dog kidney in NANBAO JIAONANG, and this method sensitivity is good, and specificity is strong, phase The feminine gender answered is noiseless, simple using equipment, easily operated.Can the true and false superiority and inferiority to NANBAO JIAONANG in the market identify.
Quality testing of the present invention to dog kidney in NANBAO JIAONANG, mainly examines following factor:
1. in the method, selection n-hexane, acetone, petroleum ether extract the effective component in dog kidney, through experiments, it was found that, petroleum Ether extraction effect is good, and colour developing is clear, noiseless.
2. specificity is tested: also containing other animal drugs, such as donkey kidney, pilose antler, hippocampus in NANBAO JIAONANG.According to test sample Solution preparation method prepares donkey kidney, pilose antler, hippocampus solution, separately takes treasure for Man test solution and reference substance dog kidney solution, respectively point sample in On same silica gel g thin-layer plate, measured by text method.The result shows that in sample chromatogram figure, comparison medicine dog kidney solution and treasure for Man Test solution near Rf value 0.5 be in indigo spot, donkey kidney, pilose antler, hippocampus sample solution with comparison medicine wood color It composes and is speckless on corresponding position.
3. negative blank control test: removing the NANBAO JIAONANG simulation prescription of dog kidney, the blank sample without dog kidney is made Negative control solution is made according to test solution preparation method in product.Test solution and reference substance solution separately are taken, is surveyed by text method It is fixed.The result shows that there is no spot on position corresponding with reference medicine chromatography in blank sample solution in sample chromatogram figure Point.It is noiseless to illustrate that negative blank measures it.
Specific embodiment
The present invention will be further explained with reference to the examples below, and the examples are merely illustrative, by no means implies that it It limits the scope of the invention in any way.This is further illustrated below by way of the detection method embodiment of dog kidney in NANBAO JIAONANG The beneficial effect of invention.The Chinese medicine that the present invention uses is by commercially available.
Embodiment 1
The preparation of NANBAO JIAONANG:
By Radix Ophiopogonis 13g, Morinda officinalis (system) 10.5g, thizoma curculiginis 13g, faenum graecum (system) 16g, cynomorium songaricum 13g, Radix Glycyrrhizae 13g, teasel root 8g, profound Join 13g, radix aconiti lateralis preparata 9.5g, radix achyranthis bidentatae 8g, Semen Cuscutae 13g, Radix Astragali (system) 30g, Rehmannia glutinosa 17g, Poria cocos 27g, Rhizoma Atractylodis Macrocephalae (system) 16.5g, Fructus Corni (system) 10g, psoralea corylifolia (system) 25g, fructus lycii 13g, Herba Cistanches (system) 9g, raspberry 13g, Herba Epimedii (system) Medicinal material extracts 26g 20 simply, is condensed into the clear cream that relative density is 1.0.
Take ginseng 25g, pilose antler 25g, hippocampus 13g, donkey kidney 30g, dog kidney 25g, Radix Angelicae Sinensis 21g, root bark of tree peony 12g, Cortex Eucommiae 20g, Ah Glue 13g, ten taste pulverizing medicinal materials fine powder of cortex cinnamomi 14.5g.Above-mentioned fine powder is uniformly mixed with clear cream, stirring granulation is dry, is packed into glue Capsule is made capsule 1000.
Detection method includes the following steps for dog kidney in its finished product.
This product content 2.0g is taken, petroleum ether 10ml is added, after ultrasonic extraction 30 minutes, centrifuging and taking supernatant is that sample is molten Liquid is measured according to thin layer chromatography, and taking sample solution 10ul point sample is the benzene-of 1:5:2:3 with volume ratio on silica gel g thin-layer plate N-hexane-acetone and ethyl acetate mixed liquor is as solvent, after 11-15cm is unfolded, takes out, dries, set ultraviolet lamp respectively Thin-layer chromatography is observed under 365nm, and 5% ethanol solution of sulfuric acid of even spraying on lamellae, 100 DEG C of heating after ten minutes, then are set Observed under daylight thin-layer chromatography;If in the chromatography of above two view mode, one of multiple spots are in Rf obtained in lamellae Value 0.5 nearby has fluorescence spot, and has color change after spraying color developing agent, is in hyacinthine, then dog renal drug material drug effect in NANBAO JIAONANG Ingredient exists.
Embodiment 2
Method of quality control of the invention not only can be as the measuring method of dog kidney in control NANBAO JIAONANG, it is also possible to as dog The regular dosage forms such as the control method of other preparations of kidney, including pill, granule, capsule, tablet.
The identification of dog kidney in the commercially viable three kidneys ball of quality control method of the invention.
Three kidney ball prescriptions: deer kidney (talcum powder scalds) 17.5g, dog kidney (talcum powder scalds) 17.5g, donkey kidney (talcum powder scalds) 17.5g, thizoma curculiginis 15g, monkshood (system) 15g, cortex cinnamomi 15g, Herba Epimedii (sheep oil toast) 17.5g, pawpaw 12g, cortex moutan 10.5g, mountain Medicine (bran stir-fry) 15g, Fructus Corni 15g, Rhizoma Atractylodis Macrocephalae (soil is fried) 15g, Poria cocos 15g, fennel seeds (salt toast) 8g, Radix Glycyrrhizae (honey toast) 8g, dried orange peel 8g, Paper mulberry Fruit (salt toast) 10g, raspberry 10.5g, teasel root 10.5g, Radix Angelicae Sinensis 8g, Rhizoma Chuanxiong 8g, glutinous rehmannia 10.5g, Rehmannia glutinosa 10.5g, Faenum graecum (salt toast) 8g, Herba Cistanches 8g, cynomorium songaricum 12.5g, Morinda officinalis 12.5g, psoralea corylifolia (salt toast) 8g, Radix Astragali (honey toast) 10.5g, Fructus lycii 10g, asparagus fern 10g, Radix Ophiopogonis 12g, radix achyranthis bidentatae 8g, Cortex Eucommiae (salt toast) 8g, Semen Cuscutae 8g, ginseng 12g, pilose antler (butter toast) 12g, hippocampus (butter toast) 12g, gekko (butter toast) 10.5g.Above-mentioned 39 taste medicinal material is made condensed pill 1000.
Detection method includes the following steps for dog kidney in three kidney balls:
This product content 2.0g is taken, petroleum ether 10ml is added, after ultrasonic extraction 30 minutes, centrifuging and taking supernatant is sample solution, Measured according to thin layer chromatography, take sample solution 10ul point sample on silica gel g thin-layer plate, with volume ratio for 1:5:2:3 benzene-just oneself Alkane-acetone and ethyl acetate mixed liquor is as solvent, after 11-15cm is unfolded, takes out, dries, set ultraviolet lamp 365nm respectively Lower observation thin-layer chromatography, and 5% ethanol solution of sulfuric acid of even spraying on lamellae, 100 DEG C of heating after ten minutes, then set daylight Lower observation thin-layer chromatography;If in the chromatography of above two view mode, one of multiple spots are in Rf value 0.5 obtained in lamellae Nearby there is fluorescence spot, and have color change after spraying color developing agent, is in hyacinthine, then dog renal drug material effective component is deposited in three kidney balls ?.

Claims (3)

1. the quality determining method of dog kidney in a kind of NANBAO JIAONANG, it is characterised in that: take this product content 2.0g, petroleum ether is added 10ml, after ultrasonic extraction 30 minutes, centrifuging and taking supernatant is sample solution, measures according to thin layer chromatography, takes sample solution 10ul Point sample on silica gel g thin-layer plate, using volume ratio for 1:5:2:3 benzene-n-hexane-acetone and ethyl acetate mixed liquor as expansion Agent after 11-15cm is unfolded, takes out, dries, set observe thin-layer chromatography under ultraviolet lamp 365nm respectively, and uniformly on lamellae Spraying 5% ethanol solution of sulfuric acid, 100 DEG C of heating after ten minutes, then set observed under daylight thin-layer chromatography;If above two watcher In the chromatography of formula, one of multiple spots obtained in lamellae have fluorescence spot near Rf value 0.5, and have face after spraying color developing agent Color change, then dog renal drug material effective component exists in NANBAO JIAONANG.
2. the quality determining method of dog kidney in NANBAO JIAONANG described in claim 1, it is characterised in that: the Chinese materia medica preparation sample is molten One of several spots obtained in liquid are in hyacinthine near Rf value 0.5, then dog renal drug material effective component exists in NANBAO JIAONANG.
3. the quality determining method of dog kidney in NANBAO JIAONANG described in claim 1, it is characterised in that: the method can be used for it His form of Chinese drug, the detection including dog renal drug material effective component in pill, granule, capsule, Tabules.
CN201711450165.9A 2017-12-27 2017-12-27 The quality determining method of dog kidney in a kind of NANBAO JIAONANG Pending CN109975469A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4132778A (en) * 1977-05-31 1979-01-02 Eli Lilly And Company Antibiotic A-32887
JP2001328941A (en) * 2000-05-22 2001-11-27 Yanai Yoshiaki Antiviral agent
CN101164586A (en) * 2006-10-18 2008-04-23 山西太行药业股份有限公司 Medicinal composition for treating sexual impotence and preparation process thereof
CN104792918A (en) * 2015-04-27 2015-07-22 天津力生制药股份有限公司 Quality detection method for donkey genital in Nanbao capsule
CN106896180A (en) * 2015-12-21 2017-06-27 九芝堂股份有限公司 A kind of detection method of Bushen Tianjing oral liquid

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4132778A (en) * 1977-05-31 1979-01-02 Eli Lilly And Company Antibiotic A-32887
JP2001328941A (en) * 2000-05-22 2001-11-27 Yanai Yoshiaki Antiviral agent
CN101164586A (en) * 2006-10-18 2008-04-23 山西太行药业股份有限公司 Medicinal composition for treating sexual impotence and preparation process thereof
CN104792918A (en) * 2015-04-27 2015-07-22 天津力生制药股份有限公司 Quality detection method for donkey genital in Nanbao capsule
CN106896180A (en) * 2015-12-21 2017-06-27 九芝堂股份有限公司 A kind of detection method of Bushen Tianjing oral liquid

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
GILLES CARMEL 等: "Composition and physical properties of lipids from plasma membranes of dog kidney", 《BIOCHIMICA ET BIOPHYSICA ACTA》 *
张贵君等: "貂鞭及其类似品的生药鉴定", 《中草药》 *
缪文曦 等: "蛇肾与狗肾的薄层色谱初步比较", 《中成药》 *

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Application publication date: 20190705