CN1959407A - Method for constructing fingerprint HPLC of Shatian pomelo, and normal fingerprint - Google Patents
Method for constructing fingerprint HPLC of Shatian pomelo, and normal fingerprint Download PDFInfo
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- CN1959407A CN1959407A CN 200610122923 CN200610122923A CN1959407A CN 1959407 A CN1959407 A CN 1959407A CN 200610122923 CN200610122923 CN 200610122923 CN 200610122923 A CN200610122923 A CN 200610122923A CN 1959407 A CN1959407 A CN 1959407A
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Abstract
A method for configurating HPLC fingerprint atlas of sand flat shaddock includes taking said shaddock sample powder; water boiling it; filtering; concentrating; adding alcohol and stewing; taking top clear liquid as test sample; carrying out HPLC analysis as using chromatographic column of Merck Lichrospher RP-18e ( f micron m, 250 x 4.0mm), linear gradient elution of 0min-50min, methanol of 30%-60%, acetic acid-water mixture of 36% and detection wavelength of 320nm to obtain HPLC atlas of said shaddock; comparing 18 batches of said atlas to obtain standard fingerprint atlas of said shaddock.
Description
Technical field
The present invention relates to the construction method of shatian pomelo (Citrus grandis (L.) 0sbeck var.shatinyu Hort.) HPLC finger-print, and the shatian pomelo standard finger-print that obtains of method thus.
Background technology
The chromatographic fingerprints of Chinese materia medica Quality Control Technology is an importance of the modernization of Chinese medicine.Chromatographic fingerprints of Chinese materia medica is realizing that the whole controlling party mask of material colony has remarkable advantages, has obtained the approval of international community.British Herbal Pharmacopoeia, India herbal medicine allusion quotation, German medicinal plant association, Canada is medicinal and fragrant plant association all receives the quality control method of finger-print.
Shatian pomelo is the fruit of rue family citrus plant Citrus grandis (L.) Osbeck var.shatinyu Hort., has clearing heat and moistening lung, relieving cough and reducing sputum effect.The present invention has made up the finger-print of shatian pomelo with the HPLC method, but utilizes the quality of HPLC finger-print overall monitor shatian pomelo.
Summary of the invention
The construction method that the purpose of this invention is to provide shatian pomelo (Citrus grandis (L.) Osbeck var.shatinyu Hort.) finger-print, and the shatian pomelo standard finger-print that obtains of method thus.
The construction method of shatian pomelo HPLC finger-print of the present invention comprises the steps:
(1) preparation of need testing solution: precision takes by weighing shatian pomelo sample powder (crossing 40 mesh sieves) 1.0g～5.0g, decoct 1～3 time, add 5～30 times of amounts of water at every turn, decoct 10min～2h at every turn, filter, it is 1.05～1.20 that filtrate is concentrated into relative density, add ethanol and make determining alcohol reach 50%～90%, leave standstill 6～48h, the leaching supernatant, with 0.45 μ m filtering with microporous membrane, filtrate is as need testing solution.
(2) HPLC analyzes: the accurate need testing solution 20 μ l sample introductions of drawing, and chromatographic condition is as follows: chromatographic column is MerckLichrospher RP-18e (5 μ m, 250 * 4.0mm); Moving phase is methyl alcohol-36% acetic acid water mixed liquid (80: 1, transfer pH to 3.0); Adopt the linear gradient elution mode: 0min → 50min, methyl alcohol: 30% → 60%, 36% acetic acid water mixed liquid: 70% → 40%; Flow velocity: 1ml/min; Detect wavelength: 320nm; Obtain shatian pomelo HPLC finger-print.
According to the method for the invention described above, by 18 batches of shatian pomelo samples are made up the HPLC finger-print and analyze comparison, find out its common characteristic peak (totally 13 peaks), obtain the standard finger-print of shatian pomelo.Retention time (the t at 13 total peaks
R) be respectively: 7.28min, 10.38min, 12.11min, 17.11min, 21.74min, 23.05min, 25.91min, 27.95min, 28.85min, 32.36min, 34.51min, 35.95min, 44.25min.They have constituted the fingerprint characteristic of shatian pomelo.
The present invention by absorption curve relatively to reach addition method qualitative, determine that the ownership of main peaks is as follows: t
RThe peak of=10.38min is naringenin, t
RThe peak of=17.11min is aurantiin, t
RThe peak of=21.74min is neohesperidin, t
RThe peak of=23.05min is Rhoifolin, t
RThe peak of=25.91min is meranzin hydrate, t
RThe peak of=27.95min is different meranzin, t
RThe peak of=35.95min is bergapten, t
RThe peak of=44.25min is the bergamot booth.
The present invention has following advantage and purposes: by having or not of total peak in the finger-print, can monitor the quality of shatian pomelo effectively, guarantee stable, the homogeneous, controlled of its quality.
The present invention is described further below in conjunction with embodiment and accompanying drawing.
Description of drawings:
Fig. 1 is a shatian pomelo standard finger-print of the present invention.Retention time (the t at each the total peak of numeral among the figure
R).
Embodiment
The preferred embodiments of the present invention are as follows:
1 instrument, sample, reagent:
1.1 instrument: DIONEX high performance liquid chromatograph (ASI-100 automatic sampler, ATH-585 column oven, P680 quaternary gradient pump, PDA-100 detecting device); HP1100 high performance liquid chromatograph (quaternary pump, online degasser, column oven, automatic sampler, DAD detecting device).Chromatographic column: Merck Lichrospher RP-18e (5 μ m, 250 * 4.0mm).
1.2 sample: 18 batches of shatian pomelo samples respectively from super flat, the Cangwu, Guangxi in Mei County, Guangdong, Guangxi, Rong County, Guangxi and other places, are the fruit of rue family citrus plant shatian pomelo Citrus grandis (L.) Osbeck var.shatinyu Hort. through evaluation.
1.3 reagent: naringenin reference substance, aurantiin reference substance (Nat'l Pharmaceutical ﹠ Biological Products Control Institute provides); Neohesperidin reference substance, Rhoifolin reference substance, bergapten reference substance (Sigma company provides); Meranzin hydrate, different meranzin, bergamot booth (modern Chinese herbal medicine quality research development centre, Zhongshan University Guangzhou provides, and purity is higher than 99.5%).Liquid-phase chromatographic analysis reagent is chromatographically pure, and it is pure that all the other reagent are analysis, and water is ultrapure water.
2 methods and result
2.1 the preparation of need testing solution: precision takes by weighing shatian pomelo sample powder (crossing 40 mesh sieves) 2.0g, decoct 3 times, add 15 times of amounts of water at every turn, decoct 1h at every turn, filter, it is 1.10～1.12 that filtrate is concentrated into relative density, add ethanol and make determining alcohol reach 80%, leave standstill 24h, the leaching supernatant, with 0.45 μ m filtering with microporous membrane, filtrate is as need testing solution.
2.2HPLC analyze: the accurate need testing solution 20 μ l sample introductions of drawing, chromatographic condition is as follows: chromatographic column is MerckLichrospher RP-18e (5 μ m, 250 * 4.0mm); Moving phase is methyl alcohol-36% acetic acid water mixed liquid (80: 1, transfer pH to 3.0); Adopt the linear gradient elution mode: 0min → 50min, methyl alcohol: 30% → 60%, 36% acetic acid water mixed liquid: 70% → 40%; Flow velocity: 1ml/min; Detect wavelength: 320nm; Obtain shatian pomelo HPLC finger-print.
2.3 determining of total peak: above-mentioned 18 batches of shatian pomelo sample HPLC finger-prints that obtain are analyzed comparison, find out its common characteristic peak (totally 13 peaks), obtain the standard finger-print of shatian pomelo.Retention time (the t at 13 total peaks
R) be respectively: 7.28min, 10.38min, 12.11min, 17.11min, 21.74min, 23.05min, 25.91min, 27.95min, 28.85min, 32.36min, 34.51min, 35.95min, 44.25min.They have constituted the fingerprint characteristic of shatian pomelo.
2.4 the evaluation of main peaks: by absorption curve relatively to reach the reference substance addition method qualitative, determined that the ownership of main peaks is as follows: t
RThe peak of=10.38min is naringenin, t
RThe peak of=17.11min is aurantiin, t
RThe peak of=21.74min is neohesperidin, t
RThe peak of=23.05min is Rhoifolin, t
RThe peak of=25.91min is meranzin hydrate, t
RThe peak of=27.95min is different meranzin, t
RThe peak of=35.95min is bergapten, t
RThe peak of=44.25min is the bergamot booth.
Claims (2)
1. the construction method of a shatian pomelo HPLC finger-print may further comprise the steps:
(1) preparation of need testing solution: precision takes by weighing shatian pomelo sample powder (crossing 40 mesh sieves) 1.0g～5.0g, decoct 1～3 time, add 5～30 times of amounts of water at every turn, decoct 10min～2h at every turn, filter, it is 1.05～1.20 that filtrate is concentrated into relative density, add ethanol and make determining alcohol reach 50%～90%, leave standstill 6～48h, the leaching supernatant, with 0.45 μ m filtering with microporous membrane, filtrate is as need testing solution;
(2) HPLC analyzes: the accurate need testing solution 20 μ l sample introductions of drawing, and chromatographic condition is as follows: chromatographic column is MerckLichrospher RP-18e (5 μ m, 250 * 4.0mm); Moving phase is methyl alcohol-36% acetic acid water mixed liquid (80: 1, transfer pH to 3.0); Adopt the linear gradient elution mode: 0min → 50min, methyl alcohol: 30% → 60%, 36% acetic acid water mixed liquid: 70% → 40%; Flow velocity: 1ml/min; Detect wavelength: 320nm; Obtain shatian pomelo HPLC finger-print;
(3) measure 18 batches of shatian pomelo sample HPLC finger-prints and comparing, obtain the shatian pomelo HPLC standard finger-print that constitutes by its total peak, the retention time (t at 13 common characteristic peaks that this finger-print has
R) be respectively: 7.28min, 10.38min, 12.11min, 17.11min, 21.74min, 23.05min, 25.91min, 27.95min, 28.85min, 32.36min, 34.51min, 35.95min, 44.25min.
2. according to the described shatian pomelo HPLC of claim 1 finger-print, it is characterized in that: t
RThe peak of=10.38min is naringenin, t
RThe peak of=17.11min is aurantiin, t
RThe peak of=21.74min is neohesperidin, t
RThe peak of=23.05min is Rhoifolin, t
RThe peak of=25.91min is meranzin hydrate, t
RThe peak of=27.95min is different meranzin, t
RThe peak of=35.95min is bergapten, t
RThe peak of=44.25min is the bergamot booth.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB200610122923XA CN100485386C (en) | 2006-10-20 | 2006-10-20 | Method for constructing HPLC fingerprint graph spectrum of Shatian pomelo |
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| CNB200610122923XA CN100485386C (en) | 2006-10-20 | 2006-10-20 | Method for constructing HPLC fingerprint graph spectrum of Shatian pomelo |
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| CN100485386C CN100485386C (en) | 2009-05-06 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103344729A (en) * | 2013-07-15 | 2013-10-09 | 西南大学 | Method for identifying authenticity and evaluating quality of Fengjie navel oranges |
| CN104316635A (en) * | 2014-10-28 | 2015-01-28 | 石河子大学 | Method for rapidly identifying flavor and quality of fruits |
| CN106442778A (en) * | 2016-09-14 | 2017-02-22 | 广西大学 | Method for identifying Shatian pomelo in Rong County of Guangxi by adopting chromatography |
| CN106442777A (en) * | 2016-09-14 | 2017-02-22 | 广西大学 | Method for identifying Fujian Guanxi honey pomelos by chromatography method |
| CN107383040A (en) * | 2017-07-05 | 2017-11-24 | 浙江大学 | A kind of method that bergamot element is isolated and purified from early fragrant shaddock oil vacuole layer |
-
2006
- 2006-10-20 CN CNB200610122923XA patent/CN100485386C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103344729A (en) * | 2013-07-15 | 2013-10-09 | 西南大学 | Method for identifying authenticity and evaluating quality of Fengjie navel oranges |
| CN104316635A (en) * | 2014-10-28 | 2015-01-28 | 石河子大学 | Method for rapidly identifying flavor and quality of fruits |
| CN106442778A (en) * | 2016-09-14 | 2017-02-22 | 广西大学 | Method for identifying Shatian pomelo in Rong County of Guangxi by adopting chromatography |
| CN106442777A (en) * | 2016-09-14 | 2017-02-22 | 广西大学 | Method for identifying Fujian Guanxi honey pomelos by chromatography method |
| CN106442777B (en) * | 2016-09-14 | 2018-11-27 | 广西大学 | A method of Fu Jian Guanxi small stream honey shaddock is identified using chromatography |
| CN106442778B (en) * | 2016-09-14 | 2019-01-29 | 广西大学 | A method of Guangxi Rong County shatian pomelo is identified using chromatography |
| CN107383040A (en) * | 2017-07-05 | 2017-11-24 | 浙江大学 | A kind of method that bergamot element is isolated and purified from early fragrant shaddock oil vacuole layer |
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| CN100485386C (en) | 2009-05-06 |
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