CN203479772U - High performance liquid chromatography fingerprint measuring device of dendrobium candidum - Google Patents
High performance liquid chromatography fingerprint measuring device of dendrobium candidum Download PDFInfo
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- CN203479772U CN203479772U CN201320368683.7U CN201320368683U CN203479772U CN 203479772 U CN203479772 U CN 203479772U CN 201320368683 U CN201320368683 U CN 201320368683U CN 203479772 U CN203479772 U CN 203479772U
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Abstract
The utility model discloses a high performance liquid chromatography fingerprint measuring device of dendrobium candidum. The measuring device sequentially comprises a test sample solution preparation device and a spectrum measuring device, wherein the spectrum measuring device comprises a high performance liquid chromatograph and an analysis chromatographic column cooperatively used together with the high performance liquid chromatograph, and the analysis chromatographic column is an ECOSIL chromatographic column. The test sample solution preparation device sequentially comprises a fourth sieve used for sieving a test sample, a balance used for weighing the mass of the sieved test sample, a conical flask used for dissolving the test sample and provided with a stopper, an ultrasonic instrument used for extracting the test sample solution, a filter used for filtering the test sample solution, and a microfiltration membrane. The ECOSIL chromatographic column is a 5 microns chromatographic column with a specification of 4.6mm*250mm. The aperture of the microfiltration membrane is 0.45 microns. The measuring device is simple and convenient to operate and is beneficial to providing reference for interspecific identification and quality evaluation of dendrobium candidum medicinal materials.
Description
Technical field
The utility model relates to pharmaceutical analysis apparatus, is specifically related to a kind of dendrobium candidum efficient liquid-phase chromatograph finger print atlas determinator.
Background technology
(the dendrobe chromatogram finger print measuring method such as Cheng Jinle, application number: 200810218494.5) disclose a kind of stem of noble dendrobium finger print measuring method, its extracting method need to extract with monohydroxy alcohol, volatilize rear constant volume, in chromatographic condition, use acetonitrile: 0.1% acetic acid is as mobile phase, and it only extracts with monohydroxy alcohol, can only make the finger-print of Alcohol soluble composition, and water soluble ingredient is also most important in the stem of noble dendrobium, this part can not show in chromatogram.A kind of (method of differentiating the dendrobium candidum true and false with HPLC finger-print such as Lv Guiyuan, application number: 201010255558.6) disclose a kind of method of differentiating the dendrobium candidum true and false with HPLC finger-print, need water or monohydroxy alcohol to extract, concentrated, organic solvent extraction, reclaims concentrated, constant volume, filter, step is comparatively loaded down with trivial details, increases experimental error.(method for building up and the standard finger-prints thereof of Guangxi dendrobium candidum HPLC finger-print such as what iron light, application number: the method for building up that 201010298226.6) discloses a kind of Guangxi dendrobium candidum HPLC finger-print, appropriate 10% ammoniacal liquor is wetting, at 85 ℃, after methyl alcohol water-bath refluxing extraction 4h, filter evaporate to dryness, use again methanol constant volume, filter, the method operation is comparatively complicated, and length consuming time.
Utility model content
The utility model object is the defect for above-mentioned prior art, a kind of dendrobium candidum efficient liquid-phase chromatograph finger print atlas determinator is provided, this determinator is easy to use, accurate, reproducible, can be dendrobium candidum medicinal material species identification and quality assessment reference is provided.
For achieving the above object, the utility model is taked following technical scheme:
A kind of dendrobium candidum efficient liquid-phase chromatograph finger print atlas determinator of the present utility model, comprise in turn need testing solution preparation facilities and collection of illustrative plates determinator, described collection of illustrative plates determinator comprises high performance liquid chromatograph and the analysis chromatographic column that coordinates described high performance liquid chromatograph to use, and described analysis chromatographic column is ECOSIL chromatographic column.
Described need testing solution preparation facilities comprises test sample sieve No. four sieves, the balance of weighed test sample quality of sieving, the tool plug conical flask that dissolves described test sample, the Ultrasound Instrument of extracting described need testing solution, the filtrator that filters described need testing solution and miillpore filters of use successively.
Described ECOSIL chromatographic column is that specification is 4.6mm * 250mm, the chromatographic column of 5 μ m.The aperture of described miillpore filter is 0.45 μ m.
The method of utilizing dendrobium candidum efficient liquid-phase chromatograph finger print atlas determinator of the present utility model to measure its collection of illustrative plates is as follows:
(1) get the about 1g of test sample dendrobium candidum powder (crossing sieve No. four), accurately weighed with balance, put in tool plug conical flask, precision adds 70% methyl alcohol 20ml, and weighed weight, with Ultrasound Instrument (power 720W, frequency 32kHz) ultrasonic extraction 30min, lets cool, more weighed weight, with 70% methyl alcohol, supply the weight losing, shake up, filter, get subsequent filtrate, with filtrator, load onto 0.45 μ m filtering with microporous membrane, obtain.
(2) HPLC chromatographiccondition: for analyzing chromatographic column, acetonitrile-water is eluent gradient wash-out, flow velocity 1.0mLmin with ECOSIL chromatographic column (4.6mm * 250mm, 5 μ m)
-1, 35 ℃ of column temperatures, detect wavelength 205nm.
(3) measure: accurately draw need testing solution 30 μ L and inject high performance liquid chromatograph, by the conditional operation of step (2), record the chromatogram of 70min.
The beneficial effects of the utility model are: utilize dendrobium candidum efficient liquid-phase chromatograph finger print atlas determinator of the present utility model to carry out collection of illustrative plates mensuration, can in dendrobium candidum HPLC finger-print, show water-soluble and Alcohol soluble composition simultaneously, this determinator is simple, convenient, and being conducive to provides reference for dendrobium candidum medicinal material species identification and quality assessment.
Accompanying drawing explanation
Fig. 1 is the structural representation of a preferred embodiment of dendrobium candidum efficient liquid-phase chromatograph finger print atlas determinator of the present utility model.
Embodiment
Below in conjunction with the drawings and specific embodiments, the utility model is described in further detail, but not as to restriction of the present utility model.
A kind of dendrobium candidum efficient liquid-phase chromatograph finger print atlas determinator of the present utility model, comprise need testing solution preparation facilities 1 and collection of illustrative plates determinator 2, the analysis chromatographic column 22 that described collection of illustrative plates determinator 2 comprises high performance liquid chromatograph 21 and coordinates high performance liquid chromatograph 21 to use, described analysis chromatographic column 22 is ECOSIL chromatographic column.Described ECOSIL chromatographic column is that specification is 4.6mm * 250mm, the chromatographic column of 5 μ m.
Described need testing solution preparation facilities 1 comprise successively test sample sieve No. four of use sieves 11, weighed test sample quality of sieving balance 12, dissolve the tool plug conical flask 13 of test sample, the Ultrasound Instrument 14 of the described need testing solution of ultrasonic extraction, filter filtrator 15 and the miillpore filter 16 of the solution of described test sample, the aperture of described miillpore filter is 0.45 μ m.
The method of utilizing dendrobium candidum efficient liquid-phase chromatograph finger print atlas determinator of the present utility model to measure its collection of illustrative plates is as follows:
(1) got the about 1g of test sample dendrobium candidum powder of No. four sieves 11, accurately weighed with balance 12, put in tool plug conical flask 13, precision adds 70% methyl alcohol 20ml, and weighed weight, with the ultrasonic extraction of Ultrasound Instrument 14 30min(power 720W, frequency 32kHz), let cool, more weighed weight, with 70% methyl alcohol, supply the weight losing, shake up, with filtrator 15 and 0.45 μ m filtering with microporous membrane 16, filter, get subsequent filtrate, with filtrator 15 and 0.45 μ m filtering with microporous membrane 16, filter, obtain.
(2) HPLC chromatographiccondition: for analyzing chromatographic column, acetonitrile-water is eluent gradient wash-out, flow velocity 1.0mLmin with ECOSIL chromatographic column (4.6mm * 250mm, 5 μ m)
-1, 35 ℃ of column temperatures, detect wavelength 205nm.
(3) measure: accurately draw need testing solution 30 μ L injection liquid chromatographies, by the conditional operation of step (2), record the chromatogram of 70min.
(4) similarity analysis: " the similarity evaluation A version " software that utilizes the Chinese Pharmacopoeia council to recommend, the similarity comparison of carrying out to gained finger-print (is set up with reference to finger-print with median, time window is 0.50), obtain the similarity of ten batches of dendrobium candidums, and set up the common pattern of dendrobium candidum principal ingredient finger-print, similarity is all greater than 0.844, Fig. 1 is that (S1-S10 is respectively dendrobium candidum NYT1～NYT10 to dendrobium candidum principal ingredient finger-print, R is the common pattern of dendrobium candidum principal ingredient finger-print), Fig. 2 is dendrobium candidum principal ingredient finger-print common pattern collection of illustrative plates, table 1 is ten batches of dendrobium candidum similarity result of calculations.Wherein, S1, S2, S3, S4, S5, S6, S7, S8, S9, S10 represent that respectively first is to the tenth batch of dendrobium candidum.R represents similarity.
This presentation of results utilizes dendrobium candidum efficient liquid-phase chromatograph finger print atlas determinator of the present utility model to carry out collection of illustrative plates mensuration, can in dendrobium candidum HPLC finger-print, show water-soluble and Alcohol soluble composition simultaneously, this determinator is simple, convenient, can provide reference for dendrobium candidum medicinal material species identification and quality assessment.
Table 1
Claims (3)
1. a dendrobium candidum efficient liquid-phase chromatograph finger print atlas determinator, comprise in turn need testing solution preparation facilities and collection of illustrative plates determinator, it is characterized in that, described collection of illustrative plates determinator comprises high performance liquid chromatograph and the analysis chromatographic column that coordinates described high performance liquid chromatograph to use, and described analysis chromatographic column is ECOSIL chromatographic column; Described need testing solution preparation facilities comprises test sample sieve No. four sieves, the balance of weighed test sample quality of sieving, the tool plug conical flask that dissolves described test sample, the Ultrasound Instrument of extracting described need testing solution, the filtrator that filters described need testing solution and miillpore filters of use in turn, and described miillpore filter is close to the filtration mouth place of described filtrator.
2. collection of illustrative plates determinator according to claim 1, is characterized in that, described ECOSIL chromatographic column is that specification is 4.6mm * 250mm, the chromatographic column of 5 μ m.
3. collection of illustrative plates determinator according to claim 1, is characterized in that, the aperture of described miillpore filter is 0.45 μ m.
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| CN201320368683.7U CN203479772U (en) | 2013-06-25 | 2013-06-25 | High performance liquid chromatography fingerprint measuring device of dendrobium candidum |
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| CN201320368683.7U CN203479772U (en) | 2013-06-25 | 2013-06-25 | High performance liquid chromatography fingerprint measuring device of dendrobium candidum |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105259269A (en) * | 2015-11-05 | 2016-01-20 | 北京蓝标一成科技有限公司 | Establishing method for dendrobe characteristic fingerprint spectrum |
| CN106680403A (en) * | 2016-12-30 | 2017-05-17 | 安徽农业大学 | Method for detecting dendrophenol in Dendrobium officinale |
| CN112858570A (en) * | 2021-01-13 | 2021-05-28 | 广东韶钢松山股份有限公司 | Method for detecting calcium content in solid calcium wire |
-
2013
- 2013-06-25 CN CN201320368683.7U patent/CN203479772U/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105259269A (en) * | 2015-11-05 | 2016-01-20 | 北京蓝标一成科技有限公司 | Establishing method for dendrobe characteristic fingerprint spectrum |
| CN105259269B (en) * | 2015-11-05 | 2017-07-14 | 北京蓝标一成科技有限公司 | A kind of method for building up of stem of noble dendrobium characteristic fingerprint pattern |
| CN106680403A (en) * | 2016-12-30 | 2017-05-17 | 安徽农业大学 | Method for detecting dendrophenol in Dendrobium officinale |
| CN112858570A (en) * | 2021-01-13 | 2021-05-28 | 广东韶钢松山股份有限公司 | Method for detecting calcium content in solid calcium wire |
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