CN107300593A - The detection method of gingerol composition in ginger and its processed product - Google Patents
The detection method of gingerol composition in ginger and its processed product Download PDFInfo
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- CN107300593A CN107300593A CN201710547636.1A CN201710547636A CN107300593A CN 107300593 A CN107300593 A CN 107300593A CN 201710547636 A CN201710547636 A CN 201710547636A CN 107300593 A CN107300593 A CN 107300593A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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Abstract
The invention discloses a kind of detection method of gingerol composition in ginger and its processed product, comprise the following steps：(1) one or more in 6 gingerols, 8 gingerols and 10 gingerol reference substances are taken, is placed in container, then heats；(2) solvent dissolving is added after cooling down, mixed reference substance solution is obtained；(3) by mixed reference substance solution injecting chromatograph, the appearance on chromatogram can realize the chromatographic peak detection and localization of gingerol composition in ginger and its processed product using the chromatogram.The present invention is promoted gingerol constituents to be changed into salad oil and zingiberone, the chromatographic peak detection and localization of a variety of gingerol compositions is realized with 13 kinds of reference substances, accurate positioning, cost is low using the chemical property of composition in itself in ginger by simple technique.
Description
Technical field
The invention belongs to traditional Chinese medicine ingredients detection technique field, it is related to a kind of inspection of gingerol composition in ginger and its processed product
Survey method.
Background technology
Ginger is zingiber Zingiber officinale Rosc. new fresh quench stem, and its traditional processed product has dry
Ginger, simmer ginger, baked ginger, ginger charcoal etc., be respectively adopted dry, simmer system (parcel scalds), scalded with husky (soil) fry to a certain degree, stir-fry charcoal etc.
Gained.《Japanese Pharmacopoeia》Record and ginger, its Cheng Wei Dry ginger are processed using the method steamed or cooked.
The chemical composition of ginger includes polysaccharide, Zingibain, flavones ingredient, gingerol constituents, volatile oil composition.
And gingerol constituents (in structure include 3- methoxyl group -4- hydroxy phenyls functional group) are as the active component generally acknowledged in ginger,
Its type includes gingerol, salad oil and zingiberone etc..
Method such as titration, gravimetric method etc. of the quantitative evaluation method rationalization analysis of conventional Chinese medicine；Instrumental Analysis
Method such as ultraviolet spectrophotometry, high performance liquid chromatography, gas chromatography etc., and the method for Instrumental Analysis is accurate fixed in realization
It is required to use standard substance (reference substance) during amount, some reference substances are due to factors such as stability, the contents of itself chemical property
Cause it to be difficult to obtain, price it is high, carry out its testing cost during multicomponent measure especially high.Realized using the method for Instrumental Analysis
During assay, there are two key factors, one is to obtain retention time realization to position the chromatographic peak of material, and two be to obtain
The response (instrument signal intensity, such as peak area, peak height, the relation with material actual concentrations) of tie substance is realized quantitative
Purpose.
The localization method of current chromatographic peak has reference substance direct location, and this method is that current positioning is the most square
Method, but because reference substance is expensive, carry out price during multicomponent measure especially high.Reference extract method, but reference extract
Preparation be difficult in itself, also needed to before use carry out reference extract in each composition demarcation, although can realize multicomponent
Determine, but cost is also higher in application.
One surveys between poor method of the relative retention time methods for commenting method to use, linear regression chromatographic peak correction method, retention time etc. more
The method for connecing positioning, the positioning of chromatographic peak is carried out by calculating, but these methods have error, in the application by chromatogram
Post, determining instrument, the equal hardware of flowing influence it is larger.Meanwhile, chromatographic peak passes through meter compared with horn of plenty in ginger class product chromatogram
Often there are multiple chromatographic peaks near obtained retention time, this method also has problem in actual applications.
The content of the invention
It is an object of the invention to：There is provided ginger in a kind of ginger and its processed product is peppery for the problem of existing for prior art
The detection method of plain composition, can realize the chromatographic peak detection and localization of a variety of gingerol compositions with 1-3 kind reference substances, and positioning is accurate
Really, cost is low.
To achieve these goals, the technical solution adopted by the present invention is：
The detection method of gingerol composition, comprises the following steps in a kind of ginger and its processed product：
(1) one or more in 6-gingerol, 8-gingerol and 10-gingerol reference substance are taken, is placed in container, then heats；
(2) container after step (1) is heated is taken out, and solvent dissolving is added after cooling, obtains containing zingiberone, gingerol simultaneously
And the positioning mixed reference substance solution of salad oil；
(3) the mixed reference substance solution injecting chromatograph for obtaining step (2), the appearance on chromatogram, utilize the chromatogram
The chromatographic peak detection and localization of gingerol composition in ginger and its processed product can be achieved in figure.
As the preferred scheme of the present invention, in the step (1), first toward adding water and closed in container before heating, addition
The ratio between the quality of water and the gross mass of reference substance are 1:1-10.
As the preferred scheme of the present invention, in the step (1), mode of heating be baking oven bake, infrared heating or microwave
Heating.
As the preferred scheme of the present invention, in the step (1), heating-up temperature is 60-220 DEG C, and the heat time is 0.5-
4h。
As the preferred scheme of the present invention, in the step (1), heating-up temperature is 120-140 DEG C, and the heat time is 2-
4h。
As the preferred scheme of the present invention, in the step (2), the solvent of addition is acetonitrile.
The beneficial effects of the present invention are：
The present invention promotes gingerol constituents to be changed into using the chemical property of composition in itself in ginger by simple technique
Salad oil and zingiberone, the chromatographic peak detection and localization of a variety of gingerol compositions are realized with 1-3 kind reference substances, and comment relative to a survey
Method positioning is more accurate, and relative to reference substance direct location, positioning is equal accurate, but reduces the species of reference substance, into
This is lower.
Therefore, accurate, the inexpensive chromatographic peak for realizing gingerol composition in the ginger and its processed product positioning of the present invention
Detection, can save the cost of ginger and its processed product quality control, convenient and swift, environmental protection and economy is widely used.
Brief description of the drawings
Fig. 1 adds acetonitrile to obtain mixed reference substance solution only to mix 6-gingerol, 8-gingerol and 10-gingerol, without reality
Example 1 is applied to handle and chromatogram that direct injection analysis is obtained；
Fig. 2 is the chromatogram that embodiment 1 is obtained；
Fig. 3 is the chromatogram that comparative example 1 is obtained.
Embodiment
In order that the object, technical solutions and advantages of the present invention are clearer, below in conjunction with accompanying drawing to the excellent of the present invention
Embodiment is selected to be described in detail.
In the present invention, gingerol composition includes zingiberone (English name zingerone), 6-gingerol (English name 6-
Gingerol), 8-gingerol (English name 8-Gingerol), 10-gingerol (English name 10-Gingerol), (E)-1-(4-hydroxy-3-methoxyphenyl)dec-4-en-3-one (English
Literary fame claims 6-Shogaol), 8- salad oils (English name 8-Shogaol) and 10- salad oils (English name 10-Shogaol).
The chromatographic condition of following examples and comparative example is：
Chromatographic column：Waters BridgeTMC18 (250 × 4.6nm, 5 μm)；Mobile phase is A phases：0.2% formic acid-water, B
Phase：0.2% formic acid-acetonitrile；Using binary gradient elutes, elution program is 0-3min, B phases 60%~60%；3-8min, B phase
60%-50%；8-10min, B phase 50%~40%；10-20min, B phase 40%~32%；20-30min, B phase 32%~
25%；30-35min, B phase 25%~5%；35-40min, B phase 5%~5%；Flow velocity：0.8mL/min；Detection wavelength：
280nm；Column temperature：30℃；Sample size：10μL.
Embodiment 1
(1) take 6-gingerol, 8-gingerol and each 0.1mg of 10-gingerol reference substance to be placed in container, then add 0.1 μ L watertights,
It is placed in 120 DEG C of baking 4h in baking oven；
(2) container after step (1) is baked is taken out, and acetonitrile dissolving is added after cooling, obtains containing zingiberone, 6- ginger simultaneously
Phenol, 8-gingerol, 10-gingerol, (E)-1-(4-hydroxy-3-methoxyphenyl)dec-4-en-3-one, the positioning mixed reference substance solution of 8- salad oils and 10- salad oils；
(3) mixed reference substance solution for obtaining step (2) sample introduction under foregoing chromatographic condition is analyzed, and is obtained such as the institute of table 4
Each composition retention time shown and chromatogram as shown in Figure 2.
The reference substance direct location of comparative example 1
(1) accurately weighed zingiberone, 6-gingerol, 8-gingerol, 10-gingerol, (E)-1-(4-hydroxy-3-methoxyphenyl)dec-4-en-3-one, 8- salad oils, 10- salad oils are fitted
Every 1mL respectively solution containing 0.1mg is respectively prepared in amount, plus acetonitrile, and mixed reference substance solution is obtained after mixing；
(2) mixed reference substance solution for obtaining step (1) sample introduction under foregoing chromatographic condition is analyzed, and is obtained such as the institute of table 4
Each composition retention time shown and chromatogram as shown in Figure 3.
The relative retention time method of comparative example 2
(1) 7 kinds of gingerol composition retention times relative to each other (horizontal seat of the brand chromatographic column of relative retention time=6 is determined
Mark the Average residence time of the ordinate composition of the brand chromatographic column of Average residence time/6 of composition), it is as shown in table 1 below：
(2) accurately weighed 6-gingerol is appropriate, plus solution of every 1mL containing 0.1mg is made in acetonitrile, obtains 6-gingerol reference substance molten
Liquid；
(3) the 6-gingerol reference substance solution for obtaining step (2) sample introduction under foregoing chromatographic condition is analyzed, and uses following public affairs
Formula calculates each composition retention time：The retention time T of composition to be measuredx=ft× T, wherein Tx are the retention time of composition to be measured, ft
For the relative retention time of composition to be measured/control composition, T is the retention time of control composition；Obtain each composition as shown in table 4
Retention time.
The retention time of comparative example 3 difference method
(1) retention time for determining 7 kinds of gingerol compositions is poor, as shown in table 2 below and table 3：
(2) accurately weighed 6-gingerol is appropriate, plus solution of every 1mL containing 0.1mg is made in acetonitrile, obtains 6-gingerol reference substance molten
Liquid；
(3) the 6-gingerol reference substance solution for obtaining step (2) sample introduction under foregoing chromatographic condition is analyzed, and uses following public affairs
Formula calculates each composition retention time：Retention time Tx=T+ the Δ T, wherein Tx of composition to be measured are the retention time of composition to be measured, T
To compare the retention time of composition, Δ T is that retention time is poor；Obtain each composition retention time as shown in table 4.
Fig. 1 adds acetonitrile to obtain mixed reference substance solution only to mix 6-gingerol, 8-gingerol and 10-gingerol, without reality
Example 1 is applied to handle and chromatogram that direct injection analysis is obtained.
By Fig. 1, Fig. 2 and Fig. 3 contrast, handled by embodiment 1, can be 6-gingerol, 8-gingerol, 10- ginger
Phenol is disposably changed into zingiberone, (E)-1-(4-hydroxy-3-methoxyphenyl)dec-4-en-3-one, 8- salad oils and 10- salad oils, while retaining original 6-gingerol, 8- ginger
Phenol, 10-gingerol, therefore on the basis of Fig. 13 kinds of composition chromatographic peaks, the chromatographic peak of 4 kinds of compositions is added, 7 kinds of compositions are in color
Peak sequence is followed successively by zingiberone, 6-gingerol, 8-gingerol, (E)-1-(4-hydroxy-3-methoxyphenyl)dec-4-en-3-one, 10-gingerol, 8- salad oils, 10- salad oils on spectrogram, respectively
It is completely the same that composition peak sequence and position and Fig. 3 reference substance directly position obtained chromatogram, and occurs without obvious impurity,
It can be seen that, embodiment 1 can realize that the chromatographic peak of 7 kinds of gingerol compositions is accurately positioned detection with 3 kinds of reference substances.
The result of table 4 shows, 7 kinds of gingerol composition retention times that the method for embodiment 1 is obtained are compareed with comparative example 1
7 kinds of gingerol composition retention times that product direct location is obtained are consistent, and a survey comments method (during the relative reservation of comparative example 2 more
Between the indirect addressing such as method, the poor method of the retention time of comparative example 3 method) data there is certain deviation, one surveys and comments method pair more
The compositions such as zingiberone, 8- salad oils, 10- salad oils can not be differentiated accurately when positioning.
To sum up, embodiment 1 realizes the chromatographic peak detection and localization of 7 kinds of gingerol compositions with 3 kinds of reference substances, and is surveyed relative to one
It is comment method positioning more accurate more, and relative to reference substance direct location, positioning is equal accurate, but reduce the kind of reference substance
Class, cost is lower.
On the basis of 7 kinds of gingerol composition chromatographic peak detection and localizations of embodiment 1, with reference to determining that a conventional survey is commented more
Amount method, according to relative correction factor, by calculating, you can to realize the quantitative determination of 7 kinds of gingerol compositions.Such as table 5 and table 6
Shown, compared with the direct measurement result of reference substance, the degree of accuracy is higher.
The present invention is that the chromatographic peak detection and localization of a variety of gingerol compositions is realized with 1-3 kind reference substances, is not limited to implement
The chromatographic peak detection and localization that 7 kinds of gingerol compositions are realized with 3 kinds of reference substances of example 1, the present invention can also be a kind or 2 kinds control
Product realize the chromatographic peak detection and localization of a variety of gingerol compositions, and it is that can be achieved to 6-gingerol, 6- zingiberenes that 6-gingerol, which is such as used alone,
The detection and localization of phenol, zingiberone.In addition, the present invention is also not limited to the application in liquid phase systems simultaneously, this method principle is at other
Also it is feasible in chromatographic system.
Finally illustrate, the above embodiments are merely illustrative of the technical solutions of the present invention and it is unrestricted, although pass through ginseng
According to the preferred embodiments of the present invention, invention has been described, it should be appreciated by those of ordinary skill in the art that can
So that various changes are made to it in the form and details, the present invention limited without departing from appended claims
Spirit and scope.
Claims (6)
1. the detection method of gingerol composition in a kind of ginger and its processed product, it is characterised in that：Comprise the following steps：
(1) one or more in 6-gingerol, 8-gingerol and 10-gingerol reference substance are taken, is placed in container, then heats；
(2) container after step (1) is heated is taken out, and solvent dissolving is added after cooling, obtains containing zingiberone, gingerol and ginger simultaneously
The positioning mixed reference substance solution of alkene phenol；
(3) the mixed reference substance solution injecting chromatograph for obtaining step (2), the appearance on chromatogram can using the chromatogram
Realize the chromatographic peak detection and localization of gingerol composition in ginger and its processed product.
2. the detection method of gingerol composition in ginger according to claim 1 and its processed product, it is characterised in that：It is described
In step (1), first toward adding water and closed in container before heating, the ratio between the quality of the water of addition and the gross mass of reference substance are 1:1-
10。
3. the detection method of gingerol composition in ginger according to claim 1 and its processed product, it is characterised in that：It is described
In step (1), mode of heating is that baking oven is baked, infrared heating or microwave are heated.
4. the detection method of gingerol composition in ginger according to claim 1 and its processed product, it is characterised in that：It is described
In step (1), heating-up temperature is 60-220 DEG C, and the heat time is 0.5-4h.
5. the detection method of gingerol composition in ginger according to claim 4 and its processed product, it is characterised in that：It is described
In step (1), heating-up temperature is 120-140 DEG C, and the heat time is 2-4h.
6. the detection method of gingerol composition in ginger according to claim 1 and its processed product, it is characterised in that：It is described
In step (2), the solvent of addition is acetonitrile.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108709788A (en) * | 2018-04-23 | 2018-10-26 | 河南科高中标检测技术有限公司 | The methods for commenting method to measure gingerol content in ginger medicinal substances extract are surveyed using one more |
| CN109470794A (en) * | 2018-12-21 | 2019-03-15 | 广东方制药有限公司 | A kind of discrimination method of stir-baked CORTEX MAGNOLIAE OFFICINALIS with rhizoma zingiberis recens juice magnolia obovata |
| CN109856261A (en) * | 2018-12-29 | 2019-06-07 | 上海市儿童医院 | A method of effective component in " point application side " is analyzed using HPLC simultaneously |
| CN110308224A (en) * | 2019-07-18 | 2019-10-08 | 成都市中草药研究所(成都市卫生计生药械科技服务中心) | A kind of method of quality control of ginger processed product |
| CN113030329A (en) * | 2021-03-15 | 2021-06-25 | 广东省科学院生物工程研究所 | One-test-multiple-evaluation method for determining content of 6 gingerol components in ginger juice brown sugar |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108709788A (en) * | 2018-04-23 | 2018-10-26 | 河南科高中标检测技术有限公司 | The methods for commenting method to measure gingerol content in ginger medicinal substances extract are surveyed using one more |
| CN109470794A (en) * | 2018-12-21 | 2019-03-15 | 广东方制药有限公司 | A kind of discrimination method of stir-baked CORTEX MAGNOLIAE OFFICINALIS with rhizoma zingiberis recens juice magnolia obovata |
| CN109856261A (en) * | 2018-12-29 | 2019-06-07 | 上海市儿童医院 | A method of effective component in " point application side " is analyzed using HPLC simultaneously |
| CN110308224A (en) * | 2019-07-18 | 2019-10-08 | 成都市中草药研究所(成都市卫生计生药械科技服务中心) | A kind of method of quality control of ginger processed product |
| CN113030329A (en) * | 2021-03-15 | 2021-06-25 | 广东省科学院生物工程研究所 | One-test-multiple-evaluation method for determining content of 6 gingerol components in ginger juice brown sugar |
| CN113030329B (en) * | 2021-03-15 | 2022-10-11 | 广东省科学院生物工程研究所 | One-test-multiple-evaluation method for determining content of 6 gingerol components in ginger juice brown sugar |
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Application publication date: 20171027 |