CN106518878A - Method for extracting folic acid from spinach leaf powder - Google Patents
Method for extracting folic acid from spinach leaf powder Download PDFInfo
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- CN106518878A CN106518878A CN201610896630.0A CN201610896630A CN106518878A CN 106518878 A CN106518878 A CN 106518878A CN 201610896630 A CN201610896630 A CN 201610896630A CN 106518878 A CN106518878 A CN 106518878A
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- folic acid
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- spinach
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D475/00—Heterocyclic compounds containing pteridine ring systems
- C07D475/02—Heterocyclic compounds containing pteridine ring systems with an oxygen atom directly attached in position 4
- C07D475/04—Heterocyclic compounds containing pteridine ring systems with an oxygen atom directly attached in position 4 with a nitrogen atom directly attached in position 2
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- Organic Chemistry (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention relates to a method for extracting folic acid from spinach leaf powder. The method comprises: (1) primary extraction of folic acid from spinach leaf powder: adding an extraction solution to a raw material spinach leaf powder, carrying out dark soaking extraction at a constant temperature, centrifugating the extraction liquid, and carrying out suction filtration to obtain a supernatant; and (2) silica gel chromatography column adsorption and separation: adsorbing the supernatant through a silica gel adsorbent, eluting with a dichloromethane-methanol solution system, collecting the separation liquid, and carrying out nitrogen blowing concentration on the tarter separation liquid to obtain the folic acid extract. According to the present invention, the method has characteristics of simple process, easy operation, and high safety.
Description
Technical field
The invention belongs to the preparation of plant extracts, and in particular to extract the side of folic acid in a kind of powder from the leaf of spinach
Method.
Background technology
Folic acid (Folic acid), also known as vitamine M or pteroylglutamic acid, is a kind of greenish orange yellow crystal or thin slice.Leaf
Acid is more stable in atmosphere, but easily decomposes so as to lose activity under illumination condition；Folic acid is in an acidic solution to hot unstable
It is fixed but relatively stable in neutral and alkaline environment.The molecular formula of folic acid is C19H19N7O6, molecular weight is 441.4；Its molecule master
If being made up of pteridine, p-aminobenzoic acid and three part of glutamic acid.
Folic acid is a kind of B family vitamins extremely important to health, can be used to synthesizing, DNA plerosis, outstanding for pregnant woman
Which is important, is effectively reduced the outbreak probability of neonate's NTD disease.However, human body itself cannot synthesize folic acid, can only
By ordinary meal or medicine Supplement of folic acid.Folic acid is mainly distributed in animal's liver, green vegetable and microorganism, wherein greenery
Vegetables are the important sources of Supplement of folic acid in people's daily life, but content it is generally relatively low and because the species of crop is different content
, therefore obtain the problem that the content of various kinds of foods Folic Acid is always Related Research Domain concern.(" the folic acid such as slow Hyosung
Extraction and Study of Antioxidation ",《Modern food science and technology》, 27 phases in 2011) and with rape, mushroom, banana as raw material, with inclined phosphorus
Acid be extractant, fluorometric determination, draw banana Folic Acid content be 38.8 μ g/g, rape be 25.2 μ g/g, mushroom
For 23.8 μ g/g；Shao Lihua etc. (" millet folic acid extracts the research with assay method ",《Food industry science and technology》, 34 phases in 2013)
It is 2.29 μ g/g equally to determine the folate content in millet.But the systematic phase for extracting folic acid from the leaf of spinach is there is no at present
Close report.
The content of the invention
It is an object of the invention to provide a kind of method for extracting folic acid from the leaf of spinach, the method simple process, it is easy to
Operation, it is safe.
Technical scheme is as follows：
A kind of method for extracting folic acid in powder from the leaf of spinach, comprises the following steps：
(1) it is preliminary from the leaf of spinach powder to extract folic acid：To in the leaf of spinach powder stock, add liquid ratio (v/m) to be 10-
20 times of extraction solution lucifuge soak extraction 10-50min at a constant temperature, leaching liquor obtain supernatant Jing after centrifugation, suction filtration；
(2) silica gel column chromatography adsorbing separation：The supernatant Jing silicagel columns adsorbent is adsorbed, methylene chloride-methanol is used
Solution system is eluted, and collects separating liquid, target separation liquid nitrogen is blown and is concentrated to give the folic acid extract.
The leaf of spinach powder in step (1) is that, from market directly purchase, mesh number is 100 mesh.
During extract solute in step (1) is phosphoric acid, potassium dihydrogen phosphate, ammonium acetate, ammoniacal liquor or NaOH
It is a kind of.
Extract solute in step (1) is ammonium acetate, and concentration is 30mmol/L.
Liquid ratio (v/m) in step (1) is 12 times, and the steady temperature is 25 DEG C or 50 DEG C or 75 DEG C or 100
DEG C constant temperature, the extraction time are 30min.
Centrifugal condition in step (1) is rotating speed 6000rpm, and centrifuging temperature is 25 DEG C, and centrifugation time is 15min.
In step (1), from the leaf of spinach powder, the preliminary folic acid that extracts is carried out in the case of lucifuge.
The mesh number of silica gel described in step (2) be 100 mesh, the model Φ 32mm*457mm of chromatographic column.
In step (2), methylene chloride-methanol proportioning is 5～7:3～5 (v/v), in silica gel column chromatography, silica gel is highly
5～15cm, supernatant loading volume are 3～8mL.
The present invention tentatively extracts the folic acid in the leaf of spinach powder using ammonium acetate solution and is further separated with silicagel column, can
The folic acid that purity is 50% or so is obtained, while yield is in 9.72 μ g/g or so.The present invention is using the leaf of spinach powder as extraction
The raw material of folic acid, cheap and easy to get and environmental protection；Using the relatively low ammonium acetate solution of toxicity as carrying that folic acid is tentatively extracted
Liquid is taken, the security of experimental implementation is improved while extraction efficiency is taken into account；Complete process is easy to operate, does not have spy to equipment
Different requirement；Show that the content of the leaf of spinach Folic Acid is about 9.72 μ g/g by the present invention simultaneously, be that respective crop Folic Acid contains
The measure of amount provides reference.
Description of the drawings
Impact of Fig. 1 solid-liquid ratios to the preliminary extraction effect of folic acid
Impact of Fig. 2 extracts solute to the preliminary extraction effect of folic acid
Impact of Fig. 3 Extracting temperatures to the preliminary extraction effect of folic acid
Impact of Fig. 4 extraction times to the preliminary extraction effect of folic acid
Specific embodiment
The present invention is conducted further description with reference to specific embodiment：
Embodiment 1
(1) it is preliminary from the leaf of spinach powder to extract folic acid：The acetic acid of 30mmol/L is added in 60g the leaf of spinach powder stocks
Ammonium salt solution 720mL, the constant temperature lucifuge soak extraction 30min under the conditions of 75 DEG C, by leaching liquor in 6000rpm, under the conditions of 25 DEG C from
Heart 15min, suction filtration obtain supernatant.
(2) silica gel column chromatography adsorbing separation：By supernatant loading 5mL, Jing 10cm high silicagel column adsorbent absorption,
Use dichloromethane:Methyl alcohol=7:3 (v/v) solution system is eluted, and collects separating liquid, target separation liquid nitrogen is blown described in being concentrated to give
Folic acid extract.
Embodiment 2
(1) it is preliminary from the leaf of spinach powder to extract folic acid：The acetic acid of 30mmol/L is added in 60g the leaf of spinach powder stocks
Ammonium salt solution 600mL, the constant temperature lucifuge soak extraction 10min under the conditions of 50 DEG C, by leaching liquor in 6000rpm, under the conditions of 25 DEG C from
Heart 15min, suction filtration obtain supernatant.
(2) silica gel column chromatography adsorbing separation：By supernatant loading 8mL, Jing 5cm high silicagel column adsorbent absorption,
Use dichloromethane:Methyl alcohol=8:2 (v/v) solution system is eluted, and collects separating liquid, target separation liquid nitrogen is blown described in being concentrated to give
Folic acid extract.
Embodiment 3
(1) it is preliminary from the leaf of spinach powder to extract folic acid：The phosphorus of 0.05mol/L is added in 60g the leaf of spinach powder stocks
Acid solution 1200mL, the constant temperature lucifuge soak extraction 50min under the conditions of 25 DEG C, by leaching liquor in 6000rpm, under the conditions of 25 DEG C from
Heart 15min, suction filtration obtain supernatant.
(2) silica gel column chromatography adsorbing separation：By supernatant loading 3mL, Jing 15cm high silicagel column adsorbent absorption,
Use dichloromethane:Methyl alcohol=6:4 (v/v) solution system is eluted, and collects separating liquid, target separation liquid nitrogen is blown described in being concentrated to give
Folic acid extract.
Embodiment 4
(1) it is preliminary from the leaf of spinach powder to extract folic acid：3% NaOH is added in 60g the leaf of spinach powder stocks
Solution 900mL, the constant temperature lucifuge soak extraction 40min under the conditions of 100 DEG C, by leaching liquor in 6000rpm, are centrifuged under the conditions of 25 DEG C
15min, suction filtration obtain supernatant.
(2) silica gel column chromatography adsorbing separation：By supernatant loading 5mL, Jing 15cm high silicagel column adsorbent absorption,
Use dichloromethane:Methyl alcohol=5:5 (v/v) solution system is eluted, and collects separating liquid, target separation liquid nitrogen is blown described in being concentrated to give
Folic acid extract.
It will be clear that the invention is not restricted to embodiment here, those skilled in the art's announcement of the invention,
The conspicuously improved and modification made by present inventive concept all should be within protection scope of the present invention.
Claims (9)
1. a kind of method for extracting folic acid in powder from the leaf of spinach, is characterized in that comprising the following steps：
(1) it is preliminary from the leaf of spinach powder to extract folic acid：To in the leaf of spinach powder stock, add liquid ratio (v/m) to be 10-20 times
Extraction solution lucifuge soak extraction 10-50min at a constant temperature, leaching liquor obtains supernatant Jing after centrifugation, suction filtration；
(2) silica gel column chromatography adsorbing separation：The supernatant Jing silicagel columns adsorbent is adsorbed, dichloro methane-methanol is used
System is eluted, and collects separating liquid, target separation liquid nitrogen is blown and is concentrated to give the folic acid extract.
2. the method for extracting folic acid in a kind of powder from the leaf of spinach according to claim 1, is characterized in that the step (1)
In the leaf of spinach powder be that, from market directly purchase, mesh number is 100 mesh.
3. the method for extracting folic acid in a kind of powder from the leaf of spinach according to claim 1, is characterized in that the step (1)
In extract solute be one kind in phosphoric acid, potassium dihydrogen phosphate, ammonium acetate, ammoniacal liquor or NaOH.
4. the method for extracting folic acid in a kind of powder from the leaf of spinach according to claim 3, is characterized in that the extract
Solute is ammonium acetate, and concentration is 30mmol/L.
5. the method for extracting folic acid in a kind of powder from the leaf of spinach according to claim 1, is characterized in that the step (1)
In liquid ratio (v/m) be 12 times, the steady temperature be 25 DEG C or 50 DEG C or 75 DEG C or 100 DEG C of constant temperatures.
6. the method for extracting folic acid in a kind of powder from the leaf of spinach according to claim 1, is characterized in that the step (1)
In centrifugal condition be rotating speed 6000rpm, centrifuging temperature be 25 DEG C, centrifugation time is 15min.
7. the method for extracting folic acid in a kind of powder from the leaf of spinach according to claim 1, is characterized in that the step (1)
In from the leaf of spinach powder the preliminary folic acid that extracts carry out in the case of lucifuge.
8. the method for extracting folic acid in a kind of powder from the leaf of spinach according to claim 1, is characterized in that the step (2)
Described in silica gel mesh number be 100 mesh, the model Φ 32mm*457mm of chromatographic column.
9. the method for extracting folic acid in a kind of powder from the leaf of spinach according to claim 1, is characterized in that the step (2)
Middle methylene chloride-methanol proportioning is 5～7:3～5 (v/v), in silica gel column chromatography, silica gel is highly 5～15cm, supernatant loading
Volume is 3～8mL.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610896630.0A CN106518878A (en) | 2016-10-14 | 2016-10-14 | Method for extracting folic acid from spinach leaf powder |
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| CN201610896630.0A CN106518878A (en) | 2016-10-14 | 2016-10-14 | Method for extracting folic acid from spinach leaf powder |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107156854A (en) * | 2017-05-19 | 2017-09-15 | 陶圣香 | A kind of preparation method of multielement folic acid |
| CN107643353A (en) * | 2016-07-20 | 2018-01-30 | 中国计量科学研究院 | Folic acid prepares purification process |
| CN110967231A (en) * | 2019-11-22 | 2020-04-07 | 北京振东康远制药有限公司 | Method for detecting folic acid content |
| CN113582996A (en) * | 2021-06-02 | 2021-11-02 | 韶关市星河生物科技有限公司 | Application of hypsizigus marmoreus strain in preparation of folic acid |
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| CN102175794A (en) * | 2011-01-13 | 2011-09-07 | 浙江大学 | Method for measuring content of total folic acid and derivatives thereof in vegetables synchronously and quantitatively |
| CN105440036A (en) * | 2016-01-05 | 2016-03-30 | 吉林省农业科学院 | Method for extracting folic acid from soybeans |
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2016
- 2016-10-14 CN CN201610896630.0A patent/CN106518878A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102175794A (en) * | 2011-01-13 | 2011-09-07 | 浙江大学 | Method for measuring content of total folic acid and derivatives thereof in vegetables synchronously and quantitatively |
| CN105440036A (en) * | 2016-01-05 | 2016-03-30 | 吉林省农业科学院 | Method for extracting folic acid from soybeans |
Non-Patent Citations (1)
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| 李小燕,等: "硅胶柱色谱分离纯化生物发酵液中叶酸的研究", 《氨基酸和生物资源》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107643353A (en) * | 2016-07-20 | 2018-01-30 | 中国计量科学研究院 | Folic acid prepares purification process |
| CN107643353B (en) * | 2016-07-20 | 2020-05-01 | 中国计量科学研究院 | Preparation and purification method of folic acid |
| CN107156854A (en) * | 2017-05-19 | 2017-09-15 | 陶圣香 | A kind of preparation method of multielement folic acid |
| CN110967231A (en) * | 2019-11-22 | 2020-04-07 | 北京振东康远制药有限公司 | Method for detecting folic acid content |
| CN110967231B (en) * | 2019-11-22 | 2022-07-08 | 北京振东康远制药有限公司 | Method for detecting folic acid content |
| CN113582996A (en) * | 2021-06-02 | 2021-11-02 | 韶关市星河生物科技有限公司 | Application of hypsizigus marmoreus strain in preparation of folic acid |
| CN113582996B (en) * | 2021-06-02 | 2024-02-06 | 韶关市星河生物科技有限公司 | Application of hypsizigus marmoreus strain in preparation of folic acid |
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