CN105067733B - A kind of ultra high efficiency closes the method that phase chromatography determines food vitamins E contents - Google Patents
A kind of ultra high efficiency closes the method that phase chromatography determines food vitamins E contents Download PDFInfo
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Abstract
The invention provides a kind of ultra high efficiency closes the method that phase chromatography determines food vitamins E contents, detailed process is：Food is carried out to extract the pretreatment of vitamin E, extract is obtained；The content that chromatography is separated and detects eight kinds of vitamin E isomers in extract respectively is closed using ultra high efficiency, respective mass concentration is obtained；Testing conditions are：Mobile phase is supercritical carbon dioxide and methanol/isopropanol (1:1) mixed liquor；The gradient elution ratio of supercritical carbon dioxide is：0 2.0min is 90% 100%, and 2.0 6.0min are 75% 85%, and 6.0 6.2min are 90% 100%；Detection wavelength is 294nm；Content is calculated by formula.The present invention can in quick separating in 7min respectively quantitative determination go out food eight kinds of vitamin E isomers content, have the advantages that detection speed is fast, separating degree is high, sensitivity is high, repeatability is good.
Description
Technical field
The present invention relates to the quantitative detection field of vitamin E, closes phase chromatography in particular to a kind of ultra high efficiency and determines
The method of food vitamins E contents.
Background technology
Vitamin E is also called tocopherol, including tocopherol and two class of tocotrienol totally 8 kinds of compounds, i.e. α, β, γ, δ
Tocopherol and α, β, γ, δ tocotrienol.Vitamin E is a kind of very high natural of activity, can protect cell membrane
And the oxidation that low-density lipoprotein causes from free radical, with preventing chronic disease, angiocardiopathy, atherosclerotic and
The function of cancer.Wherein, alpha tocopherol oxidation resistance is most strong, and studied at present is most.However, other three kinds of tocopherols are same
Sample has the unique biological characteristic for promoting health.Tocotrienols also has chemoprophylaxis and maintains neurotrophic heavy
Act on.
At present, various methods are used for the quantitative analysis of vitamin E in food and food additives, including non-aqueous capillary
Electrophoresis, high performance liquid chromatography, gas chromatography etc..In analyzing sample simultaneously, eight kinds of vitamin E isomers are mainly using height
Effect liquid phase chromatogram method, the method is topmost to have the disadvantage that analysis time length, separating degree is low, consumption of organic solvent is big.
In view of this, it is special to propose the present invention.
The content of the invention
It is an object of the invention to provide a kind of ultra high efficiency closes the method that phase chromatography determines food vitamins E contents,
Described assay method eight kinds of vitamin E isomers can contain in quick separating in 7 min respectively quantitative determination go out food
Amount, has the advantages that detection speed is fast, consumption of organic solvent is few, separating degree is high, sensitivity is high, repeatability is good.
In order to realize the above-mentioned purpose of the present invention, spy employs the following technical solutions：
A kind of ultra high efficiency closes the method that phase chromatography determines food vitamins E contents, comprises the following steps：
Quality is carried out extracting the pretreatment of vitamin E for the food of m, the extract that volume is V is obtained；
Chromatography is closed using ultra high efficiency to separate and detect containing for eight kinds of vitamin E isomers in the extract respectively
Amount, obtains respective mass concentration；Eight kinds of vitamin E isomers are：The life of α, β, γ, methyltocol and α, β, γ, δ triolefin
Educate phenol；
The ultra high efficiency closes the testing conditions of chromatography：A diameter of 3.0 mm of chromatographic column, column length are 100 mm, fill out
Material particle diameter is 1.7 μm, and filler is 2- ethylpyridine bonded silica gels；Mobile phase is supercritical carbon dioxide and methanol/isopropanol
（1:1）Mixed liquor；Using gradient elution, wherein, supercritical carbon dioxide in the percent by volume of different time sections is：0-
2.0 min are 90%-100%, and 2.0-6.0 min are 75%-85%, and 6.0-6.2 min are 90%-100%；Analysis time：4.5-
6.0 min；Column temperature：40-60℃；Standby pressure：1500-3000 psi；Sample size：0.2-10 μL；Flow velocity：1.0-3.0 mL/min；
Detection wavelength is 294 nm；
The content of eight kinds of vitamin E isomers in the food is calculated respectively by below equation：（Mass concentration *
V）/ m.
Vitamin E in food is first extracted by said determination method, is then adopted in ultra high efficiency closes chromatography
Specific elution requirement, by α, β, γ, methyltocol and α, β, γ, δ tocotrienol, this eight kinds of isomers respectively selectively divide
Match somebody with somebody, and then separate, and quantitative determination goes out its concentration.Formula is substituted into finally（Mass concentration * V）/ m, calculates eight kinds in food
The content of vitamin E isomer.Whole ultra high efficiency closes the detection process of phase chromatogram not over 7 min, and solvent load is few, and
And spectrogram show completely can be while eight kinds of vitamin E isomers be efficiently separated out.
Said determination method is applied to the various types of food of measure, for example, plant tissue（Leaf of Moringa）, fruit（It is kind wooden
Melon）And food additives（Tea oil）Deng.
Preferably, the method for the pretreatment is：
First food is beaten, adding ethanol, vitamin c solution and potassium hydroxide solution carries out saponification, obtains soap
Change product；
The saponification resultant is extracted with ether, collect extract；
The extract is dissolved with ethanol, obtain final product extract.
The preprocess method is high to the recovery rate of α, β, γ, methyltocol and α, β, γ, δ tocotrienol, and loss is few.Its
In, add vitamin c solution avoid detecting that composition is oxidized, it is high to the selectivity of vitamin E when ether is extracted, therefore use
Ether extraction can play the effect of enrichment, improve the degree of accuracy of late detection；Finally with ethanol as solvent constant volume, both can be with
Fully dissolving vitamin E, will not be interfered to follow-up chromatographic isolation again.
Preferably, when carrying out saponification, the volume ratio of ethanol, vitamin c solution and potassium hydroxide solution is 5.5-
6.5：1：1.8-2.2, and the concentration of vitamin c solution is 0.1-0.2 g/mL, the concentration of potassium hydroxide solution is 0.5-0.6
g/mL。
Using the ethanol of aforementioned proportion, vitamin C and potassium hydroxide, can be under conditions of almost zero oxygenation efficiency by food
In vitamin E fully extract, recovery rate can reach more than 90%.
Preferably, the time of the saponification is 30 more than min.
After 30 min of saponification, reaction basically reaches saturation, if extending the reaction time again, recovery rate can be improved, but phase
The cost answered can be sharply increased.
Preferably, also include before dissolving the extract with ethanol：
Distillation recovery ether.
The ether of recovery can be also used for next extraction, realize the mesh of reducing energy consumption, environmental protection detection by the step
's.
Preferably, per 1 gram of food, 8 mL potassium hydroxide solutions are at least added.
During saponification, the yield with comparison product and reaction speed between reactant has vital shadow
Ring, it is high using said ratio yield, and reaction speed is fast.
Preferably, when the food is solid-state, also included before the saponification：12 more than h of freeze-drying process.
Freeze-drying process will not both destroy detected composition, can remove water in food again, play a part of enrichment, also
The workload of later stage saponification can be reduced.
Preferably, when the ultra high efficiency closes chromatography detection：Wavelength compensation scope is 350-450 nm；The condition can
To reduce baseline noise interference, the peak type symmetry for obtaining is good, selective strong, interference is few.
Preferably, standby pressure is 1800 psi；It was found that the standby pressure of the scope, can improve the post effect of vitamin E, now separate
Best results, peak type separating degree are good.
Preferably, flow velocity is 2 mL/min.Under the conditions of being somebody's turn to do, more preferably, sensitivity is higher for separating effect.
Preferably, sampling volume be 0.8-1.2 μ L, it is ensured that peak area in more rational scope, so as to ensure
In the detection range of instrument.
Preferably, when food is solid, beating process is carried out before saponification, so that detection composition therein is discharged
Come.
Compared with prior art, beneficial effects of the present invention are：
（1）Can quickly by eight kinds of isomer separations of food vitamins E out.
（2）Quantitative determination can go out the content of eight kinds of vitamin E isomers in food respectively, and also have separating degree it is high,
The advantages of sensitivity is high, repeatability is good, detection time is short, consumption of organic solvent is few, sampling quantity is few.
（3）Improve the recovery rate of food vitamins E.
Description of the drawings【0004】
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
Accompanying drawing to be used needed for having technology description is briefly described.
Fig. 1 is the spectrogram of vitamin E reference substance in embodiment 1；
Fig. 2 is the spectrogram of sample in embodiment 1.
Specific embodiment【0005】
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the present invention.It is unreceipted concrete in embodiment
Condition person, the condition advised according to normal condition or manufacturer are carried out.Agents useful for same or the unreceipted production firm person of instrument, are
The conventional products that commercially available purchase is obtained can be passed through.
Embodiment 1
A kind of ultra high efficiency closes the method that phase chromatography determines food vitamins E contents：
First, extract：
Fresh papaya is taken, quick to be beaten, lucifuge vacuum freeze drying processes 12 h, it is then rapid to grind.Accurately weigh
12.0 g pulverized specimens sequentially add 30 mL ethanol, 5 mL vitamin Cs in 150 mL brown saponification flasks（10%, i.e. 0.1 g/
mL）With 10 mL potassium hydroxide（50%, i.e. 0.5 g/mL）Solution, flow back in boiling water bath 30 min of saponification, shakes every 8-10 min
Shake once.
Solution after saponification is cooled to room temperature, adds the ether of 85 mL to carry out extracting operation, acutely vibration 2 after sealing
Min, treats stratification, and supernatant liquid is transferred in 200 mL brown separatory funnels, second extraction is carried out with 25 mL ether,
Merge extract, and use milli-Q water extract, until eluate does not show alkalescence, discard lower floor's water phase, add appropriate anhydrous
Sodium sulphate is dried, and double-layer filter paper is filtered, and vacuum distillation is then carried out in 50 DEG C of water-baths and ether is reclaimed.Extract is filled
Point 2.0 mL ethanol are dissolved in, then 3 min are centrifuged, take supernatant, then with pin type filter filtering supernatant, the filtrate for obtaining is
Ultra high efficiency closes chromatography detection extract used.
2nd, ultra high efficiency closes chromatography bioassay standard curve：
The reference substance of α, β, γ, methyltocol and α, β, γ, δ tocotrienol is taken, a series of concentration gradients are prepared（0.1-
1.0 mg/mL）Mixed mark solution, determine content under following testing conditions, draw calibration curve.
Testing conditions：
A diameter of 3.0 mm of chromatographic column, column length are 100 mm, packing material size is 1.7 μm, and filler is 2- ethylpyridine keys
Close silica gel；Mobile phase is supercritical carbon dioxide and methanol/isopropanol（1:1）Mixed liquor；Using gradient elution, wherein, surpass
Critical carbon dioxide in the percent by volume of different time sections is：0-2.0 min are 90%-100%, and 2.0-6.0 min are 75%-
85%, 6.0-6.2 min is 90%-100%；Column temperature：50℃；Standby pressure：1800 psi；Sample size：1 μL；Flow velocity：2.0 mL/
min；Detection wavelength is 294 nm, and wavelength compensation scope is 450 nm of 350-.
3rd, ultra high efficiency closes chromatography determination sample：
Using with second step identical testing conditions Detection and Extraction liquid, obtain α, β, γ, methyltocol and α, β, γ, δ triolefin
The peak value of tocopherol, substitutes into respective calibration curve respectively, calculates concentration, then by formula（Mass concentration * V）/ m is calculated
The amount of food contained vitamin E isomer.
4th, evaluation analysis method：
Using the reappearance of identical sample evaluation said determination method, repeatability, average recovery.
The testing result of the embodiment is as follows.
（One）Eight kinds of vitamin E isomer chromatograms（Standard sample）With calibration curve respectively as shown in figure 1 and table 1.
In Fig. 1, the species and content of the isomers corresponding to label are：1- alpha tocopherols（0.999 mg/mL）, 2- δ fertilities
Phenol（0.955 mg/mL）, 3- gama tocopherols（0.475 mg/mL）, 4- β tocopherols（0.999 mg/mL）, 5- α tocotrienols
（0.4935 mg/mL）, 6- β tocotrienols（0.485 mg/mL）, 7- δ tocotrienols（0.497 mg/mL）, 8- γ triolefins
Tocopherol（0.465 mg/mL）.
The equation of linear regression and relevant parameter of 1 eight kinds of vitamin E isomer reference substances of table
Note：x：The concentration of vitamin E isomer（mg/mL）；y：Vitamin E isomer integrated peak areas；* test limit：Letter
Make an uproar ratio（S/N）For 3；* quantitative limits：Signal to noise ratio（S/N）For 10.
As it can be seen from table 1 the R of the equation of linear regression for obtaining2More than 0.9990, linear stable, error are little.
（Two）In papaya sample, vitamin E chromatogram is as shown in Figure 2；Papaya is calculated according to equation of linear regression
The content of vitamin E Isomers in sample, as shown in table 2.
In Fig. 2,1 is alpha tocopherol, and 3 is gama tocopherol.
Content of vitamin E in 2 papaya sample of table
（Three）Rate of recovery result is as shown in table 3, from table 3 it can be seen that the life of α, β, γ, methyltocol and α, β, γ, δ triolefin
The average recovery rate scope of phenol this eight kinds of vitamin E isomers is educated in 91.2%-98.2%, relative standard deviation 0.7%-3.2%.
3 recovery test of table
Embodiment 2
A kind of ultra high efficiency closes the method that phase chromatography determines food vitamins E contents：
First, extract：
2.0 g tea oils are taken, 150 mL brown saponification flasks are placed in, 27.5 mL ethanol, 5 mL vitamin Cs are sequentially added
（10%, i.e. 0.1-0.2 g/mL）With 9 mL potassium hydroxide（50%, i.e. 0.5 g/mL）Solution, flow back in boiling water bath saponification 30
Min, shakes once every 8-10 min.
Solution after saponification is cooled to room temperature, adds the ether of 85 mL to carry out extracting operation, acutely vibration 2 after sealing
Min, treats stratification, and supernatant liquid is transferred in 200 mL brown separatory funnels, second extraction is carried out with 25 mL ether,
Merge extract, and use milli-Q water extract, until eluate does not show alkalescence, discard lower floor's water phase, add appropriate anhydrous
Sodium sulphate is dried, and double-layer filter paper is filtered, and vacuum distillation is then carried out in 50 DEG C of water-baths and ether is reclaimed.Extract is filled
Point 2.0 mL ethanol are dissolved in, then 3 min are centrifuged, take supernatant, then with pin type filter filtering supernatant, the filtrate for obtaining is
Ultra high efficiency closes chromatography detection extract used.
2nd, ultra high efficiency closes chromatography bioassay standard curve：
The reference substance of α, β, γ, methyltocol and α, β, γ, δ tocotrienol is taken, one is prepared respectively to each isomers
Series standard solution, determines content under following testing conditions, draws calibration curve.
Testing conditions：
A diameter of 3.0 mm of chromatographic column, column length are 100 mm, packing material size is 1.7 μm, and filler is 2- ethylpyridine keys
Close silica gel；Mobile phase is supercritical carbon dioxide and methanol/isopropanol（1:1）Mixed liquor；Using gradient elution, wherein, surpass
Critical carbon dioxide in the percent by volume of different time sections is：0-2.0 min are 90%-100%, and 2.0-6.0 min are 75%-
85%, 6.0-6.2 min is 90%-100%；Analysis time：4.5 min；Column temperature：40℃；Standby pressure：1500 psi；Sample size：
0.2 μL；Flow velocity：1.0 mL/min；Detection wavelength is 294 nm, and wavelength compensation scope is 350-600 nm, and flow velocity is 1.0
mL/min。
3rd, ultra high efficiency closes chromatography determination sample：
Using with second step identical testing conditions Detection and Extraction liquid, obtain α, β, γ, methyltocol and α, β, γ, δ triolefin
The peak value of tocopherol, substitutes into respective calibration curve respectively, calculates concentration, then by formula（Mass concentration * V）/ m is calculated
Content of isomer in middle food.
The result of the embodiment shows that its repeatability, reappearance and the rate of recovery are consistent with embodiment 1, and can by kind
Eight kinds of vitamin E isomers in pawpaw are kept completely separate out.
Embodiment 3
A kind of ultra high efficiency closes the method that phase chromatography determines food vitamins E contents：
First, extract：
Fresh leaf of Moringa is taken, lucifuge vacuum freeze drying processes 12 h, it is then rapid to grind.12.0 g powderies are weighed accurately
Sample sequentially adds 30 mL ethanol, 5 mL vitamin Cs in 150 mL brown saponification flasks（20%, i.e. 0.2 g/mL）With 10 mL hydrogen
Potassium oxide（60%, i.e. 0.6g/mL）Solution, flow back in boiling water bath 30 min of saponification, shakes once every 8-10 min.
Solution after saponification is cooled to room temperature, adds the ether of 85 mL to carry out extracting operation, acutely vibration 2 after sealing
Min, treats stratification, and supernatant liquid is transferred in 200 mL brown separatory funnels, second extraction is carried out with 25 mL ether,
Merge extract, and use milli-Q water extract, until eluate does not show alkalescence, discard lower floor's water phase, add appropriate anhydrous
Sodium sulphate is dried, and double-layer filter paper is filtered, and vacuum distillation is then carried out in 50 DEG C of water-baths and ether is reclaimed.Extract is filled
Point 2.0 mL ethanol are dissolved in, then 3 min are centrifuged, take supernatant, then with pin type filter filtering supernatant, the filtrate for obtaining is
Ultra high efficiency closes chromatography detection extract used.
2nd, ultra high efficiency closes chromatography bioassay standard curve：
The reference substance of α, β, γ, methyltocol and α, β, γ, δ tocotrienol is taken, one is prepared respectively to each isomers
Series standard solution, determines content under following testing conditions, draws calibration curve.
Testing conditions：
A diameter of 3.0 mm of chromatographic column, column length are 100 mm, packing material size is 1.7 μm, and filler is 2- ethylpyridine keys
Close silica gel；Mobile phase is supercritical carbon dioxide and methanol/isopropanol（1:1）Mixed liquor；Using gradient elution, wherein, surpass
Critical carbon dioxide in the percent by volume of different time sections is：0-2.0 min are 90%-100%, and 2.0-6.0 min are 75%-
85%, 6.0-6.2 min is 90%-100%；Analysis time：5 min；Column temperature：60℃；Standby pressure：3000 psi；Sample size：10 μ
L；Detection wavelength is 294 nm, and wavelength compensation scope is 300-450 nm, and flow velocity is 3.0 mL/min.
3rd, ultra high efficiency closes chromatography determination sample：
Using with second step identical testing conditions Detection and Extraction liquid, obtain α, β, γ, methyltocol and α, β, γ, δ triolefin
The peak value of tocopherol, substitutes into respective calibration curve respectively, calculates concentration, then by formula（Mass concentration * V）/ m is calculated
Content of isomer in middle food.
The result of the embodiment shows that its repeatability, reappearance and the rate of recovery are consistent with embodiment 1, and can will be peppery
Eight kinds of vitamin E isomers in wooden leaf are kept completely separate out.
Although with specific embodiment illustrate and describing the present invention, but it will be appreciated that without departing substantially from the present invention's
Many other changes and modification can be made in the case of spirit and scope.It is, therefore, intended that in the following claims
Including all such changes and modifications belonged in the scope of the invention.
Claims (9)
1. a kind of ultra high efficiency closes the method that phase chromatography determines food vitamins E contents, it is characterised in that including following step
Suddenly：
Add ethanol, vitamin c solution and potassium hydroxide solution to carry out saponification to food of the quality for m, obtain saponification product
Thing；The saponification resultant is extracted with ether, collect extract；The extract is dissolved with ethanol, obtain final product volume for V's
Extract；
The content that chromatography is separated and detects eight kinds of vitamin E isomers in the extract respectively is closed using ultra high efficiency,
Obtain respective mass concentration；Eight kinds of vitamin E isomers are：The fertility of α, β, γ, methyltocol and α, β, γ, δ triolefin
Phenol；
The ultra high efficiency closes the testing conditions of chromatography：A diameter of 3.0 mm of chromatographic column, column length are 100 mm, filler grain
Footpath is 1.7 μm, and filler is 2- ethylpyridine bonded silica gels；Mobile phase is the methanol/isopropanol of supercritical carbon dioxide and grade ratio
Mixed liquor；Using gradient elution, wherein, supercritical carbon dioxide in the percent by volume of different time sections is：0-2.0 min
For 90%-100%, 2.0-6.0 min are 75%-85%, and 6.0-6.2 min are 90%-100%；Analysis time：4.5-6.0 min；Post
Temperature：40-60℃；Standby pressure：1500-3000 psi；Sample size：0.2-10 μL；Flow velocity：1.0-3.0 mL/min；Detection wavelength is
294 nm；
The content of eight kinds of vitamin E isomers in the food is calculated respectively by below equation：（Mass concentration * V）/
m。
2. ultra high efficiency according to claim 1 closes the method that phase chromatography determines food vitamins E contents, and its feature exists
In the food is selected from plant tissue, fruit.
3. ultra high efficiency according to claim 1 closes the method that phase chromatography determines food vitamins E contents, and its feature exists
In, when carrying out saponification, the volume ratio of ethanol, vitamin c solution and potassium hydroxide solution is 5.5-6.5：1：1.8-2.2,
And the concentration of vitamin c solution is 0.1-0.2 g/mL, the concentration of potassium hydroxide solution is 0.5-0.6 g/mL.
4. ultra high efficiency according to claim 3 closes the method that phase chromatography determines food vitamins E contents, and its feature exists
In the time of the saponification is 30 more than min.
5. ultra high efficiency according to claim 1 closes the method that phase chromatography determines food vitamins E contents, and its feature exists
In, with ethanol dissolving extract before also include：
Distillation recovery ether.
6. ultra high efficiency according to claim 1 closes the method that phase chromatography determines food vitamins E contents, and its feature exists
In per 1 gram of food, at least adding 8 mL potassium hydroxide solutions.
7. ultra high efficiency according to claim 1 closes the method that phase chromatography determines food vitamins E contents, and its feature exists
When, the food is solid-state, also included before the saponification：12 more than h of freeze-drying process.
8. ultra high efficiency according to claim 1 closes the method that phase chromatography determines food vitamins E contents, and its feature exists
In when the ultra high efficiency closes chromatography detection：Wavelength compensation scope is 350-450 nm.
9. ultra high efficiency according to claim 1 closes the method that phase chromatography determines food vitamins E contents, and its feature exists
In the sample size is 0.8-1.2 μ L.
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| CN106841454B (en) * | 2017-03-10 | 2019-05-10 | 国家烟草质量监督检验中心 | The chiral analysis of nicotine closes phase chromatographic tandem mass spectrography in a kind of bolete |
| CN106896175B (en) * | 2017-03-10 | 2019-04-12 | 国家烟草质量监督检验中心 | The chiral analysis of nicotine closes phase chromatographic tandem mass spectrography in a kind of Ling " for giving up smoking |
| CN107192775B (en) * | 2017-05-18 | 2019-08-23 | 中国热带农业科学院农产品加工研究所 | A kind of measuring method of determining free amino acids in food content |
| CN107290447B (en) * | 2017-06-01 | 2020-04-17 | 岛津企业管理（中国）有限公司 | Method for simultaneously detecting multiple vitamins or vitamin derivatives in infant rice flour |
| CN107367560A (en) * | 2017-07-20 | 2017-11-21 | 杭州更蓝生物科技有限公司 | A kind of ultra high efficiency closes the ascorbic method of phase chromatographic determination |
| CN107462645A (en) * | 2017-08-01 | 2017-12-12 | 河南省农业科学院芝麻研究中心 | The method of alpha tocopherol content in quick measure safflower |
| CN110596273A (en) * | 2019-09-26 | 2019-12-20 | 浙江省疾病预防控制中心 | Method for rapidly identifying natural and artificial vitamin E in health product |
| CN110988245A (en) * | 2019-12-25 | 2020-04-10 | 中储粮镇江粮油质量检测中心有限公司 | Method for rapidly detecting content of vitamin E in vegetable oil and fat and analogues thereof by ultra-high performance combined phase chromatography-mass spectrometry |
| CN113640395A (en) * | 2020-04-27 | 2021-11-12 | 深圳波顿香料有限公司 | Synthetic phase chromatographic analysis method of tocopherol acetate in electronic cigarette oil |
| CN111487356B (en) * | 2020-05-21 | 2021-11-30 | 内蒙古金达威药业有限公司 | Method for separating coenzyme Q10 by using supercritical fluid chromatography system |
| CN112526015A (en) * | 2020-11-23 | 2021-03-19 | 自然资源部第三海洋研究所 | Ultra-efficient synthetic phase chromatography for simultaneously measuring VA and VD in cod liver oil3Method (2) |
| CN115266999B (en) * | 2022-08-05 | 2024-06-18 | 陇南市祥宇油橄榄开发有限责任公司 | Qualitative and quantitative detection method for gamma-oryzanol in vegetable oil |
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