CN105116067A - Identification method for ginseng and compound preparation containing raw powder thereof - Google Patents
Identification method for ginseng and compound preparation containing raw powder thereof Download PDFInfo
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- CN105116067A CN105116067A CN201510482717.9A CN201510482717A CN105116067A CN 105116067 A CN105116067 A CN 105116067A CN 201510482717 A CN201510482717 A CN 201510482717A CN 105116067 A CN105116067 A CN 105116067A
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- ginsenoside
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Abstract
The invention relates to an identification method for ginseng and a compound preparation containing raw powder thereof. The method includes the following steps that the ginseng is subjected to ultrasonic extraction with methyl alcohol and filtered to obtain extract; the quality of the ginseng and the quality of the compound preparation containing the raw powder thereof are identified and judged by detecting ginsenoside Rg1, Re and Rf in the extract. The feed intake portion of the ginseng can be identified through the method to detect the quality of medicine containing the ginseng. In addition, the invention provides an identification method adopting ultra-high performance liquid chromatography, an ultra-high performance liquid chromatograph is used, pretreatment on a test sample is easy, and compared with a classical ginsenoside extracting method, the identification method saves manpower and material resources.
Description
Technical field
The present invention relates to the discrimination method of Chinese medicine, be specifically related to the discrimination method of ginseng and the compound preparation containing its former powder.
Background technology
Ginseng (formal name used at school: Panaxginseng), being also called Asia ginseng, is the root with meat, per nnial herb, in the theropencedrymion being grown on gentle slope, height above sea level 500-1100 rice mountain region or slope land or shaw more.Because root is loose, if shape spindle, often have bifurcated, overall picture quite like the head of people, hand, foot and four limbs, so be called ginseng.
Sweet, the micro-hardship of ginseng nature and flavor.Tepor, tonifying Qi, promoting production of body fluid and inducing sedation of the mind, beneficial gas, containing multiple saponin and polysaccharide composition, are conventional Chinese medicine.
The benefit heart relaxes and comprises series of products, and it consists of ginseng, the tuber of dwarf lilyturf, the fruit of Chinese magnoliavine, the Radix Astragali, the red sage root, Ligusticum wallichii and hawthorn.
At present, based on ginseng and higher containing the price of Ginseng Products, in order to pursue interests, some illegal businessmans adulterate, and cause the ginseng on market and as uneven in the beneficial heart product that relaxes containing its compound.
Existing method also has report to relax the discriminating of preparation or method of quality control to the beneficial heart, comprising:
CN200510038859.2 (publication number is CN1692932A) discloses a kind of preparation method and Quality Control Technology of beneficial heart relaxation grain, and Quality Control Technology is by Qualitive test and quantitative measurement ginsenoside Rg wherein
1(C
42h
72o
14) and ginsenoside Re (C
48h
82o
18) total amount, method is reliable.
CN201410566351.9 (publication number is CN104330511A) discloses a kind of beneficial heart and to relax the content assaying method of ginsenoside in preparation, it is with ginsenosides Rg1, Re and Rb1, Rc reference substance for contrast, take methyl alcohol as mobile phase A, the 0.02-2% phosphate aqueous solution high performance liquid chromatography that is Mobile phase B gradient elution.
But due to each position of ginseng herb, to contain saponin component similar, and as ginseng fibrous root, gen-seng haulms all contains ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, and content is all very high.
In order to differentiate ginseng and the true and false containing its former powder compound preparation, inventor carries out large quantifier elimination, finally proposes the present invention.
Summary of the invention
The object of this invention is to provide a kind of ginseng and the discrimination method containing its former powder compound preparation.
The invention provides a kind of method differentiating ginseng and the compound preparation quality containing its former powder, the method comprises the following steps: by ultrasonic for ginseng methyl alcohol extraction, filters, obtains extract; By ginsenoside Rg in Detection and Extraction thing
1, Re and Rf differentiate to judge the quality of ginseng and the compound preparation containing its former powder.
In said method:
Said method comprising the steps of: get ginseng 2g or get about containing the amount of ginseng raw powder 2g containing the compound preparation of its former powder, precision adds methyl alcohol 25ml, and closed ultrasonic process 60 minutes, puts to room temperature, filters, gets subsequent filtrate and get final product.
In extract, Rg
1the content that the peak area ratio of/Re is not less than 0.8, Rf should be not less than 0.03%.
Preferably, ginsenoside Rg
1the peak area ratio of/Re is (1.14-4.17), and the content of ginsenoside Rf is (0.44mg/g-0.77mg/g).
Work as Rg
1the ratio of/Re cannot calculate at about 0.2, Rf content, for ginseng fibrous root feeds intake;
Work as Rg
1the ratio of/Re cannot calculate at about 0.8, Rf content, for gen-seng haulms feeds intake;
Work as Rg
1the ratio of/Re cannot calculate at about 0.8, Rf content, and the comparision contents of Rg1 and Re is low, uses ginseng main root to feed intake but the deficiency that feeds intake.
Present invention also offers the discrimination method of a kind of ginseng and the compound preparation containing its former powder, the method comprises the following steps: the preparation of chromatographic condition, test sample, the preparation of reference substance, detection.
In above-mentioned discrimination method:
Described chromatographic condition is: adopting UPLC-UV, take octadecylsilane chemically bonded silica as filling agent (column length is 10cm, and internal diameter is 2.1mm, and particle diameter is 1.7 μm); Being mobile phase A with acetonitrile, take water as Mobile phase B; Column temperature is 30 DEG C; Flow velocity is 0.4ml per minute, and wavelength is 203nm.
Described chromatographic condition also comprises gradient elution, is specially:
| Time (minute) | Mobile phase A (%) | Mobile phase B (%) |
| 0～10 | 5～20 | 95～80 |
| 10～20 | 20 | 80 |
| 20～35 | 20～50 | 80～50 |
| 35～50 | 50～60 | 50～40 |
The preparation of described reference substance solution comprises the following steps: precision takes ginsenoside Rg1's reference substance, ginsenoside Re's reference substance and ginsenoside Rb1's reference substance, add methyl alcohol and make every 1ml respectively containing the solution of 0.8mg, precision takes ginsenoside Rf's reference substance, adds methyl alcohol and makes the solution of every 1ml containing 0.2mg.
The preparation of described need testing solution comprises the following steps: get ginseng 2g (compound preparation containing its former powder is got about containing the amount of ginseng raw powder 2g), put in tool plug conical flask, precision adds methyl alcohol 25ml, close plug, ultrasonic process 60 minutes, puts to room temperature, filter, get subsequent filtrate and get final product.
Concrete, described discrimination method comprises the following steps:
1) preparation of reference substance: precision takes ginsenoside Rg1's reference substance, ginsenoside Re's reference substance and ginsenoside Rb1's reference substance, add methyl alcohol and make every 1ml respectively containing the solution of 0.8mg, precision takes ginsenoside Rf's reference substance, adds methyl alcohol and makes the solution of every 1ml containing 0.2mg.
2) preparation of need testing solution: get ginseng 2g or get about containing the amount of ginseng raw powder 2g containing the compound preparation of its former powder, put in tool plug conical flask, precision adds methyl alcohol 25ml, close plug, and ultrasonic process 60 minutes, puts to room temperature, filters, gets subsequent filtrate and get final product;
3) chromatographic condition:
Described chromatographic condition is: adopt UPLC-UV, take octadecylsilane chemically bonded silica as filling agent, column length is 10cm, and internal diameter is 2.1mm, and particle diameter is 1.7 μm; Be mobile phase A with acetonitrile, take water as Mobile phase B, carry out gradient elution by the regulation in table 1; Column temperature is 30 DEG C; Flow velocity is 0.4ml per minute, and wavelength is 203nm,
Table 1: gradient elution
4) detect: accurate absorption reference substance solution and each 10 μ l of need testing solution respectively, injection liquid chromatography, measures, to obtain final product.
In discrimination method provided by the invention, find through detecting:
In content: ginsenoside Rg1 (C
42h
72o
14) and ginsenoside Re (C
48h
82o
18) total amount must not be less than 0.24%, ginsenoside Rb1 (C
54h
92o
23) must not 0.16% be less than, ginsenoside Rg
1the content that the peak area ratio of/Re is not less than 0.8, Rf should be not less than 0.03%.(content limit is all with the gauge that feeds intake of ginseng raw powder in compound preparation)
In foregoing thing, the content of ginsenoside Rg1 and Rb1 converts by 80% containing regulation under quantifier according to " Chinese Pharmacopoeia " version in 2010 ginseng crude drug.
Preferably:
Ginsenoside Rg
1the peak area ratio of/Re is preferably (1.14-4.17);
The content of ginsenoside Rf is preferably (0.44mg/g-0.77mg/g).
Discrimination method provided by the invention has the following advantages:
1, utilize the 87 each batch sample of this method to " the beneficial heart relaxes " series of products to measure, result shows:
1) most sample ginsenoside Rg
1the peak area ratio of/Re is about 0.2, and the content of ginsenoside Rf is extremely low cannot calculate, and infers that this sample segment uses ginseng fibrous root to feed intake.
2) a few sample ginsenoside Rg
1the peak area ratio of/Re is about 0.8, and the content of ginsenoside Rf is extremely low cannot calculate, and the content of ginsenoside Rg1 and Re exceeds standards of pharmacopoeia, because ginseng bud causes vomitting property, infers that this sample segment uses gen-seng haulms to feed intake.
3) a few sample ginsenoside Rg
1the peak area ratio of/Re is being greater than 0.8, and the content of ginsenoside Rf meets bound requirements, infers that this sample segment uses ginseng main root to feed intake.
4) a few sample ginsenoside Rg
1the peak area ratio of/Re is about 0.8, and the content of ginsenoside Rf is extremely low cannot calculate, and the comparision contents of ginsenoside Rg1 and Re is low, infers that this sample segment uses ginseng main root to feed intake but inventory wretched insufficiency.
In a word, method provided by the invention can identify the position that ginseng feeds intake, thus detects the quality containing ginseng medicine.
2, in discrimination method provided by the invention, adopt Ultra Performance Liquid Chromatography instrument, test sample pre-treatment is simple, compared with classical ginsenoside extracting method, saves manpower, material resources.
Embodiment
Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.
Embodiment 1: detection method
Measure according to high performance liquid chromatography (annex VI D).
Chromatographic condition and system suitability adopt UPLC-UV, take octadecylsilane chemically bonded silica as filling agent (column length is 10cm, and internal diameter is 2.1mm, and particle diameter is 1.7 μm); Be mobile phase A with acetonitrile, take water as Mobile phase B, carry out gradient elution by the regulation in table 2; Column temperature is 30 DEG C; Flow velocity is 0.4ml per minute, and wavelength is 203nm.
Table 2: gradient elution
| Time (minute) | Mobile phase A (%) | Mobile phase B (%) |
| 0～10 | 5～20 | 95～80 |
| 10～20 | 20 | 80 |
| 20～35 | 20～50 | 80～50 |
| 35～50 | 50～60 | 50～40 |
Precision takes ginsenoside Rg1's reference substance, ginsenoside Re's reference substance and ginsenoside Rb1's reference substance, and add methyl alcohol and make every 1ml respectively containing the solution of 0.8mg, precision takes ginsenoside Rf's reference substance, adds methyl alcohol and makes the solution of every 1ml containing 0.2mg.
The preparation of need testing solution: get ginseng 2g (compound preparation containing its former powder is got about containing the amount of ginseng raw powder 2g), put in tool plug conical flask, precision adds methyl alcohol 25ml, close plug, and ultrasonic process 60 minutes, puts to room temperature, filters, gets subsequent filtrate and get final product.
Determination method is accurate respectively draws reference substance solution and each 10 μ l of need testing solution, injection liquid chromatography, measures, to obtain final product.
Embodiment 2: existing method
Detect according to the Detection of content of ginseng content under beneficial Xinshu capsule item in Pharmacopoeia of the People's Republic of China version in 2010.
Embodiment 3:
Found by literature search and pilot study, ginseng main root and ginseng fibrous root all have ginsenoside Rf, but in ginseng fibrous root, ginsenoside Rf's content is lower.
Therefore be main differential point with ginsenoside Rf, adopt the assay method of the embodiment of the present invention 1 to detect, ginseng medicine materical crude slice and " the beneficial heart relaxes " series of samples are detected, finds ginsenoside Rg in sample
1the peak area ratio of/Re and ginseng main root gap are comparatively large, Simultaneously test ginseng fibrous root, reed head and cauline leaf, and the concrete data that detect are shown in and refer to table 3-5.
Table 3 ginseng main root measurement result
| Ginseng is originated | Lot number | Rf(mg/g) | Rg 1/Re |
| Anguo | — | 0.63 | 4.16 |
| Generation one | — | 0.77 | 3.47 |
| Sichuan lotus pond | — | 0.56 | 2.56 |
| Bozhou | 130716 | 0.57 | 4.12 |
| Bozhou | 130717 | 0.44 | 1.14 |
| Anguo | — | 0.55 | 4.17 |
Table 4 ginseng fibrous root measurement result
| Numbering | Lot number | Rf(mg/g) | Rg 1/Re |
| 1 | — | / | 0.18 |
| 2 | — | / | 0.21 |
| 3 | — | / | 0.34 |
| 4 | — | / | 0.24 |
Other Site Determination results of table 5 ginseng
| Originate in position | Lot number | Rf(mg/g) | Rg 1/Re |
| Cauline leaf 1 | — | / | 0.57 |
| Cauline leaf 2 | — | / | 0.61 |
| Reed 1 | — | / | 0.85 |
| Reed 2 | — | / | 0.80 |
("-" represents note; Represent that content is too low without "/" cannot calculate)
The result display of table 3-5: in ginseng main root, the peak area ratio of ginsenoside Rg1/Re is not less than 0.8, and the content being preferably 1.14-4.17, Rf should be not less than 0.03%, is preferably 0.44mg/g-0.77mg/g.
Although above with general explanation, embodiment and test, the present invention is described in detail, and on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, all belong to the scope of protection of present invention.
Claims (10)
1. a discrimination method for ginseng and the compound preparation containing its former powder, the method comprises the following steps: by ultrasonic for ginseng methyl alcohol extraction, filters, obtains extract; By ginsenoside Rg in Detection and Extraction thing
1, the ratio of Re and the content of Rf differentiates the quality judging ginseng and the compound preparation containing its former powder.
2. discrimination method according to claim 1, is characterized in that, get ginseng 2g or get about containing the amount of ginseng raw powder 2g containing the compound preparation of its former powder, precision adds methyl alcohol 25ml, and closed ultrasonic process 60 minutes, puts to room temperature, filters, gets subsequent filtrate and get final product.
3. discrimination method according to claim 1, is characterized in that, Rg
1the content that the peak area ratio of/Re is not less than 0.8, Rf should be not less than 0.03%.
4. discrimination method according to claim 3, is characterized in that, ginsenoside Rg
1the peak area ratio of/Re is (1.14-4.17), and the content of ginsenoside Rf is (0.44mg/g-0.77mg/g).
5. a discrimination method for ginseng and the compound preparation containing its former powder, this discrimination method comprises chromatographic condition, the preparation of need testing solution, the preparation and determination methods of reference substance solution.
6. discrimination method according to claim 5, is characterized in that, described chromatographic condition is: adopt UPLC-UV method, take octadecylsilane chemically bonded silica as filling agent, column length is 10cm, and internal diameter is 2.1mm, and particle diameter is 1.7 μm; Being mobile phase A with acetonitrile, take water as Mobile phase B; Column temperature is 30 DEG C; Flow velocity is 0.4ml per minute, and wavelength is 203nm.
7. discrimination method according to claim 6, is characterized in that, also comprises gradient elution, be specially in described chromatographic condition:
8. discrimination method according to claim 5, it is characterized in that, the preparation of described need testing solution comprises the following steps: get ginseng 2g or get the amount containing ginseng raw powder 2g containing the compound preparation of ginseng raw powder, put in tool plug conical flask, precision adds methyl alcohol 25ml, close plug, ultrasonic process 60 minutes, put to room temperature, filter, get subsequent filtrate and get final product.
9. the discrimination method according to any one of claim 5-8, is characterized in that, this discrimination method specifically comprises the following steps:
1) preparation of reference substance: precision takes ginsenoside Rg1's reference substance, ginsenoside Re's reference substance and ginsenoside Rb1's reference substance, add methyl alcohol and make every 1ml respectively containing the solution of 0.8mg, precision takes ginsenoside Rf's reference substance, adds methyl alcohol and makes the solution of every 1ml containing 0.2mg;
2) preparation of need testing solution: get ginseng 2g or get about containing the amount of ginseng raw powder 2g containing the compound preparation of its former powder, put in tool plug conical flask, precision adds methyl alcohol 25ml, close plug, and ultrasonic process 60 minutes, puts to room temperature, filters, gets subsequent filtrate and get final product;
3) chromatographic condition:
Described chromatographic condition is: adopt UPLC-UV, take octadecylsilane chemically bonded silica as filling agent, column length is 10cm, and internal diameter is 2.1mm, and particle diameter is 1.7 μm; Be mobile phase A with acetonitrile, take water as Mobile phase B, carry out gradient elution by the regulation in table 1; Column temperature is 30 DEG C; Flow velocity is 0.4ml per minute, and wavelength is 203nm,
Table 1: gradient elution
4) detect: accurate absorption reference substance solution and each 10 μ l of need testing solution respectively, injection liquid chromatography, measures, to obtain final product.
10. according to the discrimination method of any one of claim 5-8, it is characterized in that, ginsenoside Rg1 (C
42h
72o
14) and ginsenoside Re (C
48h
82o
18) total amount must not be less than 0.24%, ginsenoside Rb1 (C
54h
92o
23) must not 0.16% be less than, ginsenoside Rg
1the content that the peak area ratio of/Re is not less than 0.8, Rf should be not less than 0.03%; Ginsenoside Rg
1the peak area ratio of/Re is preferably (1.14-4.17), and the content of ginsenoside Rf is (0.44mg/g-0.77mg/g).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109709223A (en) * | 2018-12-28 | 2019-05-03 | 杭州师范大学 | The extraction detection method of saponin(e active component in a kind of folium panacis japonici cum caule |
Citations (1)
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| CN1692932A (en) * | 2005-04-11 | 2005-11-09 | 安徽科创中药天然药物研究所有限责任公司 | Method for preparing traditional Chinese medicine |
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2015
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1692932A (en) * | 2005-04-11 | 2005-11-09 | 安徽科创中药天然药物研究所有限责任公司 | Method for preparing traditional Chinese medicine |
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| YING SHI ET AL.: "Simultaneous Determination of Ten Ginsenosides in American Ginseng Functional Foods and Ginseng Raw Plant Materials by Liquid Chromatography Tandem Mass Spectrometry", 《FOOD ANAL. METHODS》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109709223A (en) * | 2018-12-28 | 2019-05-03 | 杭州师范大学 | The extraction detection method of saponin(e active component in a kind of folium panacis japonici cum caule |
| CN109709223B (en) * | 2018-12-28 | 2021-07-20 | 杭州师范大学 | Extraction and detection method of saponin active ingredients in ginseng leaves |
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