CN1811412A - Method for measuring ginger utilizing 6-gingerol oxime and 6-gingerol in products thereof - Google Patents
Method for measuring ginger utilizing 6-gingerol oxime and 6-gingerol in products thereof Download PDFInfo
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Abstract
The present invention relates to a method that can be used for qualitatively determing 6-gingeroloxime formed by means of oxime-removing reaction of 6-gingeroloxime and uses 6-gingeroloxime as internal standard of determination to determine gingerol content in fresh ginger and its products.
Description
Technical field
The present invention relates to the dietotherapeutic material---the assay method of effective constituent in ginger and the goods thereof.
Background technology
Ginger (Zingiber officinal Roscoe) is vegetables, a flavouring commonly used, be again that the Chinese crude drug of using always (comprises fresh ginger juice, CORTEX ZINGIBERIS RHIZOMAE, and the stewing ginger after concocting, ginger charcoal etc. all are the traditional Chinese medical science medicines commonly used of curing the disease), can boundary drive hundred heresies, cold, the preventing or arresting vomiting delivered, loose, effect such as reduce phlegm.Because of its " but vegetables, can and, can fruit, but medicine, its profit rich ", " Dragon Lord book on Chinese herbal medicine through " classified it as top grade, the extractum zingiberis liquidum that continent pharmacopeia and Taiwan pharmacopeia are all recorded, ginger tincture remain the stomach trouble good medicine of widely using at present.China's folklore has proverbs such as " eat three ginger morning, be better than the Ginseng Decoction ", " eat radish evening and early eat ginger, write out a prescription without the doctor ".The summary of testing for these medicine cuisine canons just, China Ministry of Public Health is defined as the dietotherapeutic resource with ginger.Modern scientific research has confirmed that these health cares of ginger or drug action all have direct or indirect relation with gingerol.The eighties in 20th century, external pharmacological testing is verified, isolated thick gingerol energy stimulating mucosal, promote gastric secretion, in enteron aisle, can suppress abnormal fermentation, promote gaseous emission, cerebral cortex and vasomotor center there are excitation, can promote blood circulation.Up-to-date experiment and clinical observation confirm: many-sided biologically actives such as gingerol has cardiac stimulant, reducing blood lipid, prevents and treats angiocardiopathy, anti-oxidant, anti-ageing, antifatigue, antitumor, preventing or arresting vomiting, relieving fainting, inhibition prostaglandin are synthetic, anticorrosion desinsection, expelling parasite, cosmetology.According to these biologically actives of gingerol, can develop the multiple flavouring, health food, medicine, the cosmetics that are applicable to different crowd, can also develop environment friendly agricultural or the like.
Gingerol (gingerol) is the spicy substance in the ginger, also is the main bioactive ingredients of ginger, and it comprises 6-gingerol (1), kind of composition (see figure 1) surplus the 8-gingerol (2), 10-gingerol (3), 12-gingerol (4) etc. ten, the character of these compositions, structure are similarly, and C is all arranged in its molecular structure
3-carbonyl and C
5-hydroxyl, this makes that the chemical property of gingerol is extremely unstable.For example, under acid condition, C
4Active hydrogen very easily with C
5Hydroxyl dewater together and form ginger brain (Shogaol); Under heating or alkali condition, C
4And C
5Between carbon-carbon bond break to form zingiberone (Zingerone) and corresponding aldehyde (see figure 1).In addition, the content of gingerol is few, only is the 2%-3% of ginger dry weight.Because gingerol poor stability in the ginger, kind is many, content is few, therefore, is not easy to mensuration.China also perfect national standard of neither one measures accurately to the gingerol in ginger and the system thereof.
In scientific research, people use the content of gingerol in titrimetry, photometry, stripping voltammetry minute and the goods thereof, but these methods all are the gingerol total amounts of measuring, and because of being subjected to the influence of background material in ginger or the ginger goods, make measurement result usually higher, the actual content with gingerol differs greatly sometimes.It is the requirement that main effective constituent is produced products such as medicine and health food that its analysis result can not satisfy with gingerol.
Because the boiling point height of gingerol own is difficult to vaporization, therefore, can not adopt the gas chromatography determination gingerol; Can obtain the gingerol derivant that can volatilize by silanization or acetylation, but still standard specimen and be difficult to accurately measure gingerol because of the derivant that forms is complicated for want of.In fact, almost had no talent this method of employing at present.
But high pressure lipuid chromatography (HPLC) normal temperature is measured, and can reduce the variation of gingerol in the mensuration process to greatest extent, is assay method relatively preferably.Yet, the qualitative gingerol standard specimen that needs of gingerol chromatographic peak not only, and know that according to the quantitative theory of stratographic analysis interior mark (or external standard) working curve when measuring gingerol, relative quantification correction factor etc. need be that prerequisite is measured with the phenol standard specimen all.Therefore, this assay method still is subjected to the restriction of gingerol standard specimen.
In a word, because the gingerol poor stability, standard specimen is rare, can't carry out accurately the gingerol in ginger and the goods thereof at present, fast measuring.
Gingerol oxime is the gingerol analog, and CN 1680290A is to the production method of gingerol oxime analogs such as 6-gingerol oxime and be used as detailed description.De-oxime reaction can take place and form the 6-gingerol in wherein described 6-gingerol oxime under certain conditions, can be used as the standard specimen that qualitatively or quantitatively determines the 6-gingerol, but up to the present, does not also have the exploration of this respect.
Summary of the invention
Purpose of the present invention just provides the method that a kind of 6-of application gingerol oxime fast, is accurately measured 6-gingerol content in ginger and the goods thereof.
The objective of the invention is to be achieved through the following technical solutions: the 6-gingerol that forms with 6-gingerol oxime de-oxime reaction carries out qualitative determination, and marks as in measuring with the 6-gingerol oxime, thereby measures the gingerol content in ginger and the goods thereof.
Specifically comprise the steps:
The sample preparation of A, ginger and goods thereof: measured object is dissolved in the mixed liquor of acetonitrile and acetic acid and is mixed with sample solution; And in this sample solution, add the 6-gingerol oxime as interior mark;
B, the 6-gingerol oxime is dissolved in the mixed liquor of acetonitrile and acetic acid, under 40～80 ℃ of temperature, reacted 10～72 hours behind the mixing, generate the 6-gingerol, and with the high pressure liquid chromatography figure of high-pressure liquid phase chromatograph measuring 6-gingerol and 6-gingerol oxime, as the qualitative determination standard substance;
C, with the high pressure liquid chromatograph peak area of 6-gingerol and 6-gingerol oxime in the working sample respectively;
D, calculate 6-gingerol content in the measured object by following formula:
C＝1.051?X?fi?As?C0/A0…………………………①
In the formula: C: the 6-gingerol concentration in institute's test sample product;
X: extension rate;
The molar absorptivity ratio of fi:6-gingerol oxime during with 6-gingerol 282nm as the relative correction factor of the two, gets 1.181 herein herein;
As: the peak area of 6-gingerol in the sample;
C0: the concentration of 6-gingerol oxime in the sample;
A0: the peak area of 6-gingerol oxime in the sample;
1.051: calculate by 6-gingerol oxime molecular weight/6-gingerol molecular weight=309/294.
In order better to realize the present invention, in the described A step, when handling the sample of ginger and goods thereof, the mass concentration of utilizing the acetonitrile of 2 volumes and 3 volumes is that 2% acetic acid mixed liquor extracts, dilution, constant volume, after being made into the sample solution that contains 0.2 gram fresh ginger/ml, the 6-gingerol oxime that adds 1～10 microgram/ml again is as interior mark.
In the described B step, take by weighing 1～20 milligram of 6-gingerol oxime, be dissolved in the 1ml acetonitrile, add 2% NaHCO3 solution 1.5ml, reacted 12～15 hours in 50～60 ℃ of baking ovens of mixing postposition.
In the described C step, the high-pressure liquid phase chromatograph measuring condition is: moving phase: 2% acetic acid mixed liquor of the acetonitrile of 2 volumes and 3 volumes; Flow velocity: 1～2mL/min; Chromatographic column: anti-phase [C18] post 4.6mm * 25cm; Column temperature: 30 ℃; Ultraviolet detection wavelength 282nm.
The present invention utilizes under the 6-gingerol oxime normal temperature and presents the crystalline powdery state, and the characteristic of preserving easily and using is used the interior mark of 6-gingerol oxime when measuring, and can measure the content of 6-gingerol in ginger and the goods thereof quickly and accurately, has wide practical value.
Description of drawings
Fig. 1 is gingerol resolves into ginger brain or zingiberone under different condition a variation synoptic diagram.
Fig. 2 is the high pressure liquid chromatography figure of 6-gingerol.
Fig. 3 is the high pressure liquid chromatography figure of 6-gingerol oxime.
Fig. 4 is the high pressure liquid chromatography figure that measures 6-gingerol in the fresh ginger.
Embodiment
Embodiment one: the mensuration of 6-gingerol in the fresh ginger
1, the processing of sample
Fresh ginger is cleaned, behind the slitting, puts in the hollander and pull an oar.Take by weighing 1.000 gram ginger slurries, utilize 2 volumes of acetonitrile and 3 volumes, 2% acetic acid mixed liquor, it is settled to 10ml, promptly be made into the sample solution of 0.200 gram fresh ginger/ml.It is put the mixing that vibrates in the Soniprep, centrifugal in 3000 rotating speeds, get supernatant and filter with 0.22 μ m nylon leaching film.Filtrate promptly can be used as the sample of measuring 6-gingerol in the fresh ginger.Sample size 2 microlitres.
In the sample of being prepared, add 5 microgram 6-gingerol oximes as interior mark.
2, the condition of high-pressure liquid phase chromatograph measuring
Sample size during mensuration is 2 microlitres.Moving phase: 2% acetic acid mixed liquor of the acetonitrile of 2 volumes and 3 volumes; Flow velocity: 1～2mL/min; Chromatographic column: anti-phase [C
18] post 4.6mm * 25cm; Column temperature: 30 ℃; Ultraviolet monitoring wavelength 282nm.Write down the peak area of 6-gingerol peak area and 6-gingerol oxime respectively.
3, the 6-gingerol is qualitative
Take by weighing 5～20 milligrams of 6-gingerol oximes, be dissolved in the 1ml acetonitrile, add 2% NaHCO
3Solution 1.5ml reacted 12～15 hours in the rearmounted 60 ℃ of baking ovens of mixing.6-gingerol oxime in this reactant liquor becomes the 6-gingerol, carries out qualitative with this 6-gingerol that reacts production.The high pressure liquid chromatography figure that measures 6-gingerol and 6-gingerol oxime according to above-mentioned condition is respectively Fig. 2 and Fig. 3.
4, the calculating of 6-gingerol mensuration and content thereof in the fresh ginger
The high pressure liquid chromatography figure of the 6-gingerol of being surveyed by above-mentioned fresh ginger sample is Fig. 4.The content that calculates the 6-gingerol according to 1. formula is: 0.09 ± 0.041% (n=3).
Embodiment two: the mensuration of 6-gingerol in the oleoresin ginger
1, the processing of sample
Take by weighing oleoresin ginger 0.1000 gram, be settled to 5ml, promptly be mixed with every milliliter of sample solution that contains 0.02 gram oleoresin ginger with 2 volumes of acetonitrile and 3 volumes, 2% acetic acid mixed liquor.It is put the mixing that vibrates in the Soniprep, centrifugal in 10000 rotating speeds, get supernatant and filter with 0.22 μ m nylon leaching film.Filtrate promptly can be used as the sample of measuring 6-gingerol in the fresh ginger.
2, the condition of high-pressure liquid phase chromatograph measuring: with embodiment one.
3, the 6-gingerol is qualitative: with embodiment one.
4, the calculating of 6-gingerol content in ginger and the goods thereof
The content that calculates the 6-gingerol according to 1. formula is: 4.01 ± 0.18% (n=3).
The mensuration of 6-gingerol in embodiment three rhizoma zingiberis
1, the processing of sample
Take by weighing 1.000 gram rhizoma zingiberis,, put the mixing that vibrates in the Soniprep with 10 milliliters of 2% acetic acid mixed liquors of the acetonitrile of 2 volumes and 3 volumes, centrifugal in 3000～10000 rotating speeds, get supernatant and filter with 0.22 μ m nylon leaching film.Be settled to 100 milliliters with the acetonitrile of 2 volumes and 2% acetic acid mixed liquor of 3 volumes.In the sample of being prepared, add 500 microgram 6-gingerol oximes as interior mark.
2, the condition of high-pressure liquid phase chromatograph measuring: with embodiment one.
3, the 6-gingerol is qualitative: with embodiment one.
4, the calculating of 6-gingerol content in ginger and the goods thereof:
The content that calculates the 6-gingerol according to 1. formula is: 0.22 ± 0.016% (n=3).
Claims (5)
1, a kind of method of utilizing the 6-gingerol oxime to measure the 6-gingerol in ginger and the goods thereof, it is characterized in that: the 6-gingerol that forms with 6-gingerol oxime de-oxime reaction carries out qualitative determination, and with the 6-gingerol oxime as mark in measuring, thereby measure gingerol content in ginger and the goods thereof.
2, method according to claim 1 is characterized in that comprising the steps:
The sample preparation of A, ginger and goods thereof: measured object is dissolved in the mixed liquor of acetonitrile and acetic acid and is mixed with sample solution; And in this sample solution, add the 6-gingerol oxime as interior mark;
B, the 6-gingerol oxime is dissolved in the mixed liquor of acetonitrile and acetic acid, under 40～80 ℃ of temperature, reacted 10～72 hours behind the mixing, generate the 6-gingerol, and with the high pressure liquid chromatography figure of high-pressure liquid phase chromatograph measuring 6-gingerol and 6-gingerol oxime, as the qualitative determination standard substance;
C, with the high pressure liquid chromatograph peak area of 6-gingerol peak area and 6-gingerol oxime in the working sample respectively;
D, calculate 6-gingerol content in the measured object: C=1.051 X fi As C0/A0 by following formula;
In the formula: C: the 6-gingerol concentration in institute's test sample product;
X: extension rate;
The molar absorptivity ratio of fi:6-gingerol oxime during with 6-gingerol 282nm as the relative correction factor of the two, gets 1.181 herein herein;
As: the peak area of 6-gingerol in the sample;
C0: the concentration of 6-gingerol oxime in the sample;
A0: the peak area of 6-gingerol oxime in the sample;
1.051: calculate by 6-gingerol oxime molecular weight/6-gingerol molecular weight=309/294.
3, method according to claim 2, it is characterized in that: in the described A step, when handling the sample of ginger and goods thereof, the mass concentration of utilizing the acetonitrile of 2 volumes and 3 volumes is that 2% acetic acid mixed liquor extracts, dilution, constant volume, after being made into the sample solution that contains 0.2 gram fresh ginger/ml, the 6-gingerol oxime that adds 1～10 microgram/ml again is as interior mark.
4, method according to claim 2 is characterized in that: in the described B step, take by weighing 1～20 milligram of 6-gingerol oxime, be dissolved in the 1ml acetonitrile, add 2%NaHCO3 solution 1.5ml, reacted 12～15 hours in 50～60 ℃ of baking ovens of mixing postposition.
5, method according to claim 2 is characterized in that: described high-pressure liquid phase chromatograph measuring condition is: moving phase: 2% acetic acid mixed liquor of the acetonitrile of 2 volumes and 3 volumes; Flow velocity: 1～2mL/min; Chromatographic column: anti-phase [C18] post 4.6mm * 25cm column temperature: 30 ℃; Ultraviolet monitoring wavelength 282nm.
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| CNB2005101206290A CN100395549C (en) | 2005-12-16 | 2005-12-16 | Method for measuring ginger utilizing 6-gingerol oxime and 6-gingerol in products thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102680637A (en) * | 2012-06-08 | 2012-09-19 | 桂林三金药业股份有限公司 | Quality detection method of gingerol type extract |
| CN104447260A (en) * | 2014-11-20 | 2015-03-25 | 广东产品质量监督检验研究院 | Method of producing gingerol by gingerol oxime |
| CN107300593A (en) * | 2017-07-06 | 2017-10-27 | 成都市中草药研究所(成都市卫生计生药械科技服务中心) | The detection method of gingerol composition in ginger and its processed product |
| CN108414665A (en) * | 2018-04-23 | 2018-08-17 | 河南科高中标检测技术有限公司 | The assay method of gingerol content in a kind of ginger medicinal material and its preparation |
| CN108414666A (en) * | 2018-04-23 | 2018-08-17 | 河南科高中标检测技术有限公司 | The assay method of gingerol content in a kind of ginger medicinal material extractive of volatile oil |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2289420C2 (en) * | 2001-11-26 | 2006-12-20 | Финцельберг Гмбх Унд Ко. Кг | Ginger extract-based preparation |
| WO2003099752A1 (en) * | 2002-05-27 | 2003-12-04 | Toagosei Co., Ltd. | Gingerol analogues and use thereof |
| CN100447129C (en) * | 2005-01-31 | 2008-12-31 | 暨南大学 | Oximated ginger phenol and its synthesis and use |
-
2005
- 2005-12-16 CN CNB2005101206290A patent/CN100395549C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102680637A (en) * | 2012-06-08 | 2012-09-19 | 桂林三金药业股份有限公司 | Quality detection method of gingerol type extract |
| CN104447260A (en) * | 2014-11-20 | 2015-03-25 | 广东产品质量监督检验研究院 | Method of producing gingerol by gingerol oxime |
| CN107300593A (en) * | 2017-07-06 | 2017-10-27 | 成都市中草药研究所(成都市卫生计生药械科技服务中心) | The detection method of gingerol composition in ginger and its processed product |
| CN108414665A (en) * | 2018-04-23 | 2018-08-17 | 河南科高中标检测技术有限公司 | The assay method of gingerol content in a kind of ginger medicinal material and its preparation |
| CN108414666A (en) * | 2018-04-23 | 2018-08-17 | 河南科高中标检测技术有限公司 | The assay method of gingerol content in a kind of ginger medicinal material extractive of volatile oil |
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