CN101419189B - HPCE fingerprint identification method for origin ginseng protection - Google Patents
HPCE fingerprint identification method for origin ginseng protection Download PDFInfo
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- CN101419189B CN101419189B CN2008100797901A CN200810079790A CN101419189B CN 101419189 B CN101419189 B CN 101419189B CN 2008100797901 A CN2008100797901 A CN 2008100797901A CN 200810079790 A CN200810079790 A CN 200810079790A CN 101419189 B CN101419189 B CN 101419189B
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Abstract
The invention provides a method for identifying HPCE fingerprints for protecting ginseng of origin, which is characterized by comprising the following steps: A, establishing fingerprints of the ginseng of origin, namely using the ginseng in the same habitat as a standard, analyzing the ginseng by capillary cataphoresis and establishing fingerprints of the cataphoresis; and B, detecting a sample, namely taking a ginseng sample to be detected, detecting the sample under the same conditions as the standard respectively to obtain a spectrogram of the detected sample, and analyzing the fingerprints of the detected sample and the standard by a direct observational method or fingerprints software as qualitative basis. The method has the advantages of simple processes, short period and low consumption; chemical information of the fingerprints of the ginseng medicinal material is comparatively rich; and the obtained characteristic peak can easily identify habitat and category of the ginseng, so as to provide reference for quality control of the origin ginseng medicinal material. The research of methodology shows that instrument precision and sample stability and repeatability of the methodhave better application prospect, so the method is suitable for popularization in the technical field of drug safety check.
Description
Technical field
The present invention relates to a kind of HPCE fingerprint discrimination method that is used for origin ginseng protection, belong to the capillary electrophoresis analysis technical field.
Background technology
Genseng is a per nnial herb, belongs to the dry root of Araliaceae.The main root meat, cylindrical or spindle, fibrous root is elongated; Root-like stock (reed head) is short, on stem trace (reed bowl) and bud bud are arranged.Genseng mainly originates in the big Xiaoxinanlin Mountains and Changbai Mountain.Wherein, the ginseng quality of producing with Changbaishan area especially is more excellent.But because different, the concocting method difference of geographical environment of genseng kind and growth causes price difference very big, so differentiate that the true and false, the quality of genseng are the task of top priority.The genseng of artificial growth is commonly referred to as " garden ginsent " at present; Garden ginsent is stung into cellular back soak, just be called " white ginseng " after drying with syrup; Immature wild ginseng transplanted in the field or immature garden ginsent transplanted and form long genseng in hill and be called " mountain ginseng ".Still do not have at present the GB of origin ginseng and recommend discrimination method, the genseng detection method that report is arranged mainly is the analysis and research of high performance liquid chromatography, with Zorbax SB-C18 chromatographic column, do moving phase at 203nm with acetonitrile-water and carry out gradient elution, indicate 18 total peaks in ginseng crude drug's finger-print altogether, and the similarity result of 10 batches of ginseng crude drug's spectrograms is calculated.The major defect of this method is: the finger-print of high-efficient liquid phase chromatogram technique analysis genseng, it is less to detect the material that separates, only the content from composition provides difference, there is not the fingerprint region in the place of production separately, and this assay method more complicated, analytical cycle is long, consumptive material expense height, and chromatographic column is easily polluted and is not easy and cleans.
Summary of the invention
The object of the present invention is to provide a kind ofly can significantly show the fingerprint region, step is simple, and the cycle is short, expends lowly, detects the Capillary Electrophoresis detection method of origin ginseng finger-print accurately.
Technical scheme of the present invention is achieved in that this HPCE fingerprint discrimination method that is used for origin ginseng protection, it is characterized in that comprising the steps:
A, set up the origin ginseng finger-print
Genseng with the same place of production is standard items, sets up its electrophoresis fingerprint by capillary electrophoresis analysis;
B, test sample
Get identical with the standard items respectively condition of samples of Ginseng to be detected and detect, draw the spectrogram of test sample, with both finger-print with direct observational method or finger-print software analysis as qualitative foundation.
The described HPCE fingerprint discrimination method that is used for origin ginseng protection is characterized in that comprising the steps:
A, the standard items genseng is carried out pre-treatment: with ginseng crude drug 60 ℃ of dry 4h in baking oven, pulverize, sieve and collect the following fine powder of 80mesh, weighing 3.0g adds 80% ethanolic solution hot reflux and extracts 2 times, each 3h, natural filtration behind the merging filtrate, behind the rotary evaporation, secondary adds water and is settled to 10mL then, 12h is placed at sombre place, get supernatant liquor, 0.22 μ m cellulose membrane filters, and filtrate is as need testing solution;
B, deposition condition:
Separating column: 75cm * 75 μ m, the not capillary column having coated layer of effective length 65cm;
Buffer solution: 20mmol/L borax soln; Organic additive: 1% aqueous solution of urea;
Detect wavelength: 243nm; Separation voltage: 18KV; Capillary temperature: 18～22 ℃ of room temperatures;
Input mode: pneumatic sample introduction;
Sample injection time: 3S;
Sample introduction pressure: 8KPa;
Purge gas: air;
C, finger-print are set up: press the standard items test solution of A step preparation, press B step deposition condition and measure, the electrophoretogram that record major constituent peak and total peak occur within 30min is demarcated 36 characteristic peaks.
D, get identical with the standard items respectively condition of commercially available samples of Ginseng and handle and measure, draw the electrophoretogram of test sample, both finger-prints are compared both finger-prints are compared to take a decision as to whether identical product.
Methodological investigation
The selection of A, object of reference:
Get standard items L-lysine and dissolve the back constant volume in volumetric flask with ultrapure water, be mixed with the standard solution that concentration is 2.5 μ mol/L, filter with aperture 0.22 μ m cellulose membrane, carry out the efficient capillary electrophoresis apparatus analysis according to the above-mentioned steps deposition condition, according to the retention time at the electrophoresis peak of L-lysine standard model as qualitative standard.With genseng standard solution and the 1:1 mixing by volume of L-lysine standard solution, carry out the efficient capillary electrophoresis apparatus analysis according to above-mentioned deposition condition simultaneously, peak height is increased qualitative method and is determined that No. 2 peaks are L-lysine.Because No. 2 peaks (L-lysine peak) separate well with adjacent component, therefore conduct is with reference to the peak.
The mensuration of B, method precision:
Get the same need testing solution of the sun-dried garden ginsent in Changbai Mountain, according to above-mentioned experiment condition, the relative migration time and relative peak height value of 8 major constituent peaks with respect to the internal standard compound peak is calculated wherein in replicate determination 5 times, the results are shown in Table 1, and finger-print is seen Fig. 2.
The test result of table 1 instrument precision
The result shows that the RSD of peak height is 1.9%～3.4% relatively, and the RSD of relative migration time is 1.4%～2.3%, shows that precision is good.
C, method reappearance are measured:
Get sun-dried transplanting mountain, Changbai Mountain and join five parts in same sample, press the 1-B experiment condition, the relative migration time and relative peak height value of 8 major constituent peaks with respect to the internal standard compound peak is calculated wherein in every part of respectively replicate determination 5 times, the results are shown in Table 2, and finger-print is seen Fig. 1.
The reproducible test result of table 2 method
The result shows that the RSD of peak height is 1.2%～2.8% relatively, and the RSD of relative migration time is 1.7%～3.3%, and the illustration method reappearance is good.
D, sample stability are measured:
Go bail for and decide the same need testing solution of the sun-dried garden ginsent of pharmacy, according to the 1-B experiment condition, respectively 0,4,8,12,24h replicate determination 2 times, calculate wherein the relative migration time and relative peak height value of 8 major constituent peaks with respect to the internal standard compound peak, the results are shown in Table 3, finger-print is seen Fig. 3.
The test result of table 3 sample stability
The result shows that the RSD of peak height is 1.1%～3.5% relatively, and the relative migration time is that RSD is 1.3%～3.1%, and interpret sample is stable in 24h at least.
The present invention adopts the capillary zone electrophoresis method that genseng has been carried out finger-print research, step is simple, cycle is short, expend low, ginseng crude drug's finger-print chemical information of setting up is abundanter, the characteristic peak that obtains is easy to distinguish the place of production, the kind of genseng, can be the control of origin ginseng quality of medicinal material reference is provided.Investigation through methodology shows: its instrument precision and sample stability and reappearance all have application promise in clinical practice, are suitable for promoting in drug safety detection technique field.
Description of drawings
Fig. 1 is the HPCE finger-print (place of production: the Changbai Mountain) of sun-dried transplanting mountain ginseng
Fig. 2 is the HPCE finger-print (place of production: the Changbai Mountain) of sun-dried garden ginsent
Fig. 3 is the HPCE finger-print (source: Baoding pharmacy) of sun-dried garden ginsent
Fig. 4 is the HPCE finger-print (source: the Changbai Mountain) of white ginseng
Fig. 5 is the HPCE finger-print (source: Liaoning) of sun-dried garden ginsent
Fig. 6 is the HPCE finger-print (source: Jilin) of sun-dried garden ginsent
Embodiment
Listed examples of the present invention is intended to further illustrate this concrete operations of HPCE fingerprint discrimination method and the application direction that is used for origin ginseng protection, and scope of the present invention is not constituted any restriction.
1, sets up the origin ginseng finger-print
A, be that standard items are made the HPCE finger-print with the sun-dried transplanting mountain on Changbai Mountain, commercially available place of production ginseng
Genseng carries out pre-treatment: with ginseng crude drug 60 ℃ of dry 4h in baking oven, pulverize, sieve and collect the following fine powder of 80mesh, weighing 3.0g adds 80% ethanolic solution hot reflux and extracts 2 times, each 3h, natural filtration behind the merging filtrate, behind the rotary evaporation, secondary adds water and is settled to 10mL then, 12h is placed at sombre place, get supernatant liquor, 0.22 μ m cellulose membrane filters, and filtrate is as need testing solution;
B, deposition condition:
Separating column: 75cm * 75 μ m, the not capillary column having coated layer of effective length 65cm;
Buffer solution: 20mmol/L borax soln; Organic additive: 1% aqueous solution of urea;
Detect wavelength: 243nm; Separation voltage: 18KV; Capillary temperature: 18～22 ℃ of room temperatures;
Input mode: pneumatic sample introduction;
Sample injection time: 3S;
Sample introduction pressure: 8KPa;
Purge gas: air;
C, finger-print are set up: the standard items test solution of pressing the preparation of A step, press B step deposition condition and measure (replicate determination 5 times, reappearance is well good), the record wherein electrophoretogram that occurs within 30min of electrophoretogram record major constituent peak and total peak is demarcated 36 characteristic peaks as shown in Figure 1.
2, sample detection
Get other commercially available 5 kinds of samples of Ginseng: the Changbai Mountain transplants that garden ginsent, Baoding pharmacy purchase that genseng, Changbai Mountain are joined in vain, garden ginsent is transplanted in Liaoning, Jilin is transplanted garden ginsent (genseng of artificial growth is commonly referred to as " garden ginsent "; Garden ginsent is stung into cellular back soak, just be called " white ginseng " after drying with syrup; Immature wild ginseng transplanted in the field or immature garden ginsent transplanted and form long genseng in hill and be called " mountain ginseng ", because different, the concocting method difference of geographical environment of their kind and growth, chemical constitution has very big-difference.) identical with standard items respectively condition handles and measure, and draws the electrophoretogram of detected sample, as Fig. 2, Fig. 3, Fig. 4, Fig. 5, shown in Figure 6.Both finger-print range estimations are compared, be easy to distinguish the place of production, the kind of genseng, can be the control of origin ginseng quality of medicinal material reference is provided.
As shown in Table 5, different ginseng crude drugs are owing to the different differences that cause its main chemical compositions of geographical environment, weather conditions, kind and concocting method of growing.Though key component content is higher than origin ginseng on the contrary in the breed of some the treated mistake ginseng, total component is many not as what originate in, and this method can well detect genseng, for the control of origin ginseng quality of medicinal material provides reference.
The different place of production of table 5 genseng finger-print testing result
Claims (1)
1. a HPCE fingerprint discrimination method that is used for origin ginseng protection is characterized in that comprising the steps:
One, sets up the origin ginseng finger-print
Genseng with the same place of production is standard items, sets up its electrophoresis fingerprint by capillary electrophoresis analysis;
Two, test sample
Get identical with the standard items respectively condition of samples of Ginseng to be detected and detect, draw the spectrogram of test sample, with both finger-print with direct observational method or finger-print software analysis as qualitative foundation;
Concrete steps comprise:
A, the standard items genseng is carried out pre-treatment: with ginseng crude drug 60 ℃ of dry 4h in baking oven, pulverize, sieve and collect the following fine powder of 80mesh, weighing 3.0g adds 80% ethanolic solution hot reflux and extracts 2 times, each 3h, natural filtration behind the merging filtrate, behind the rotary evaporation, secondary adds water and is settled to 10mL then, 12h is placed at sombre place, get supernatant liquor, 0.22 μ m cellulose membrane filters, and filtrate is as need testing solution;
B, deposition condition:
Separating column: 75cm * 75 μ m, the not capillary column having coated layer of effective length 65cm;
Buffer solution: 20mmol/L borax soln; Organic additive: 1% aqueous solution of urea;
Detect wavelength: 243nm; Separation voltage: 18KV; Capillary temperature: 18～22 ℃ of room temperatures;
Input mode: pneumatic sample introduction;
Sample injection time: 3S;
Sample introduction pressure: 8KPa;
Purge gas: air;
C, finger-print are set up: press the standard items test solution of A step preparation, press B step deposition condition and measure, the electrophoretogram that record major constituent peak and total peak occur within 30min is demarcated 36 characteristic peaks;
D, get identical with the standard items respectively condition of commercially available samples of Ginseng and handle and measure, draw the electrophoretogram of test sample, both finger-prints are compared to take a decision as to whether identical product.
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| CN101419189B true CN101419189B (en) | 2011-12-28 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1470876A (en) * | 2002-07-25 | 2004-01-28 | 浙江大学 | Chinese medicine quality control and evaluation method |
| KR20040034354A (en) * | 2003-06-12 | 2004-04-28 | (주)바이오피아 | The development of marker and analysis system for quality certification of origin |
| US6803215B1 (en) * | 2000-11-03 | 2004-10-12 | The Chinese University Of Hong Kong | Sequence characterized amplified region (SCAR) test for the authentication of traditional Chinese medicinal materials |
| CN1858582A (en) * | 2005-09-28 | 2006-11-08 | 沈百华 | Microchemical identifying method for wild ginseng and cultivated gineeng |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6803215B1 (en) * | 2000-11-03 | 2004-10-12 | The Chinese University Of Hong Kong | Sequence characterized amplified region (SCAR) test for the authentication of traditional Chinese medicinal materials |
| CN1470876A (en) * | 2002-07-25 | 2004-01-28 | 浙江大学 | Chinese medicine quality control and evaluation method |
| KR20040034354A (en) * | 2003-06-12 | 2004-04-28 | (주)바이오피아 | The development of marker and analysis system for quality certification of origin |
| CN1858582A (en) * | 2005-09-28 | 2006-11-08 | 沈百华 | Microchemical identifying method for wild ginseng and cultivated gineeng |
Non-Patent Citations (3)
| Title |
|---|
| 刘训红等.太子参的毛细管电泳指纹图谱研究.《南京中医药大学学报》.2007,第23卷(第4期),238-240. * |
| 姜先刚等.人参水溶性蛋白SDS-聚丙烯酰胺凝胶电泳指纹图谱研究.《药物分析杂志》.2008,第28卷(第6期),873-876. * |
| 李仕海等.太子参药材的HPCE指纹谱分析.《时珍国医国药》.2007,第18卷(第4期),820-821. * |
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