CN103852367B - In a kind of food, vitamin A detects the extraction process method analyzed - Google Patents
In a kind of food, vitamin A detects the extraction process method analyzed Download PDFInfo
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- CN103852367B CN103852367B CN201410123455.2A CN201410123455A CN103852367B CN 103852367 B CN103852367 B CN 103852367B CN 201410123455 A CN201410123455 A CN 201410123455A CN 103852367 B CN103852367 B CN 103852367B
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Abstract
The invention belongs to fine chemistry industry and extract field, particularly in a kind of food, vitamin A detects the extraction process method analyzed.First foodstuff samples is carried out freeze drying to remove moisture, again cryodesiccated foodstuff samples is added chloroform alcohol mixed liquor and high-speed homogenization, again that homogenised sample is centrifugal and collect the chloroform extracted solution being positioned at lower floor, add ethanol after drying up extract with nitrogen and make vitamin A redissolution purifying, adopt ultrasound wave hydrotropy in redissolution step, dissolve to make vitamin A and extract completely.Extraction of the present invention does not need the process such as alkali lye saponification degrease and decompression distillation in classic method, also overcome the foodstuff samples added existing for anhydrous sodium sulfate grinding water suction to dewater the problem such as not exclusively, there is easy and simple to handle, time shorten, extraction efficiency high, also overcoming application ether or normal hexane or methyl alcohol is the danger of Extraction solvent.Water-soluble due to ethanol, has minor amount of water even if thus extract in sample, also can not have an impact to result.
Description
Technical field
The invention belongs to fine chemistry industry and extract field, particularly in a kind of food, vitamin A detects the extraction process method analyzed.
Background technology
Vitamin A is rich content in the food such as animal's liver, fish-egg, full milk, cream, birds, beasts and eggs, with the highest in beef liver, sheep liver, is usually dissolved in the lipid material of food.Not containing established vitamin A in plant, but containing carotenoid, wherein sub-fraction carotenoid can change into vitamin A in humans and animals body, so be otherwise known as provitamin A or provitamin A.
Fat-soluble due to vitamin A, from food lipid material, extraction and isolation is out by it to select suitable solvent and method, it is the key link of determination and analysis vitamin A, moisture in food also can affect fully contacting of Extraction solvent and lipid material, thus hinder vitamin A from the extraction and isolation lipid material, therefore in food, Fat and moisture is the key factor affecting vitamin A extraction efficiency.
In current detection food in vitamin A method, first foodstuff samples is added appropriate alkaline liquor to carry out saponification process, fat in sample is combined with alkali formed saponified, and removes lipid material through washing except soap, then with ether, the vitamin A in non-saponified sample is extracted.By ether extracted liquid after anhydrous sodium sulfate elimination residual moisture, first be placed in decompression distillation in rotary evaporator and remove most of ether, obtain vitamin A extract after drying up remaining ether with nitrogen again, finally with ethanol, vitamin A extract is carried out dissolving and purify and upper machine testing.This method needs first foodstuff samples to be carried out saponification process, extract with ether again, also need to carry out processed and carry out dissolving with ethanol purifying to ether extracted liquid, there is leaching process complexity, used time is longer, easily causes many deficiencies such as the Oxidative demage of vitamin A.
In order to avoid the adverse effect of saponification process, also there is method to eliminate the process of saponification, adopt and add anhydrous sodium sulfate by sample, carry out the moisture grinding to absorb in sample at mortar, then repeatedly extract with ether or normal hexane.By extract after nitrogen dries up, then dissolve purification of vitamin A with methyl alcohol and upper machine testing.Although this kind of method eliminates saponification process, the moisture removal deposited in the sample to which is incomplete, and therefore can affect the deficiency of the organic solvents such as ether to vitamin A extraction efficiency.And in the method for application at present, be all adopt ether or normal hexane or methyl alcohol as Extraction solvent, there is Extraction solvent toxicity large, volatile, easily human body is produced to the danger of damage.
Summary of the invention
The present invention is directed to deficiency of the prior art, provide vitamin A in a kind of food to detect the extraction process method analyzed.
Technical scheme of the present invention is:
In food, vitamin A detects the extraction process method analyzed, and comprises following processing step:
Step 1: sample freeze drying: get appropriate foodstuff samples freeze drying 2-10 hour, make the residual moisture content in sample be less than 2%;
Step 2: chloroform alcohol is extracted:
1) add the chloroform alcohol mixed liquor of 10-30 times of volume in the sample after freeze drying, described chloroform alcohol mixed liquor is that chloroform and ethanol mix according to volume ratio 2:1;
2) sample is smashed homogenate completely and lucifuge lixiviate 2 hours, add physiological saline, with vortex mixer 2800 turns/min, shake 30 seconds, the protein denaturation in sample solution is separated out;
3), after concussion mixing, 4 DEG C, 3000 turns/min, centrifugal 5min, collects lower floor's chloroform extracted solution; Again repeat to extract once to remaining sample residue with described chloroform alcohol mixed liquor, extracted twice liquid is merged;
Step 3: ethanol redissolution purifying:
1) test tube will be placed in containing above-mentioned merging extract, under 26 DEG C of water bath condition, dry up with nitrogen;
2) in the test tube dried up, add ethanol in proper amount, with vortex mixer 1500 turns/min, shake 30 seconds;
3) above-mentioned ethanol extract is moved to another test tube, after drying up with nitrogen, again add ethanol in proper amount redissolution purifying;
4) machine testing on ethanol in proper amount redissolution liquid is got.
On the basis of above scheme, when in step 1, foodstuff samples is solid, first foodstuff samples cleans, and dries, and cutting into thickness is that the sheet bulk of 0.3-0.5cm carries out freeze drying again.
The invention has the beneficial effects as follows:
The steps such as in food provided by the invention, vitamin A detects the extraction process method analyzed, and its technological process mainly comprises sample freeze drying, and chloroform alcohol is extracted, ethanol redissolution purifying.First foodstuff samples is carried out freeze drying to remove moisture by the present invention, again cryodesiccated foodstuff samples is added chloroform alcohol mixed liquor and high-speed homogenization, again that homogenised sample is centrifugal and collect the chloroform extracted solution being positioned at lower floor, add ethanol after drying up extract with nitrogen and make vitamin A redissolution purifying, adopt ultrasound wave hydrotropy in redissolution step, dissolve to make vitamin A and extract completely.Extraction of the present invention does not need the process such as alkali lye saponification degrease and decompression distillation in classic method, also overcome the foodstuff samples added existing for anhydrous sodium sulfate grinding water suction to dewater the problem such as not exclusively, there is easy and simple to handle, time shorten, extraction efficiency high, also overcoming application ether or normal hexane or methyl alcohol is the danger of Extraction solvent.Water-soluble due to ethanol, has minor amount of water even if thus extract in sample, also can not have an impact to result.
Embodiment
The specific embodiment of the present invention is as follows:
Embodiment 1:
1, cutting and grinding are cleaned: take tap water and clean the pork liver 100mg dried and be placed in 15mL test tube, freeze drying 2 hours in freeze drier, makes the residual moisture content in sample be less than 2%.
2, chloroform alcohol is extracted:
1) 3mL chloroform alcohol mixed liquor (chloroform: ethanol=2:1) is added in the sample after freeze drying.
2) with high-speed homogenization machine 8000 turns/min, homogenate 2min, smashes pork liver completely and fully mixes with solvent.Lucifuge lixiviate, after 2 hours, adds 1mL physiological saline, with vortex mixer 2800 turns/min, shakes 30 seconds.
3), after concussion mixing, refrigerated centrifuge 4 DEG C, 3000 turns/min, centrifugal 5min, takes off layer chloroform extracted solution and adds in another clean 10mL test tube.
4) in remaining sample residue, add 3mL chloroform alcohol mixed liquor again repeat to extract once, extracted twice liquid is merged.
3, ethanol redissolution purifying:
1) test tube containing above-mentioned merging extract is placed in 26 DEG C of water-baths, dries up with nitrogen.
2) in the test tube dried up, add 1.5mL ethanol, with vortex mixer 1500 turns/min, shake 30 seconds, redissolve and purification of vitamin A.
4, upper machine testing:
Move in another test tube by this vitamin A alcohol solution, under same 26 DEG C of water bath condition, nitrogen dries up.The above-mentioned test tube that dries up is added 500 μ L ethanol, with vortex mixer 1500 turns/min, shakes 30 seconds, and with ultrasonic echography 30 second, vitamin A is fully dissolved; Get machine testing on 20 μ l.
Adopt the three kinds of methods mentioned in literary composition respectively to carry out extraction and analysis 5 times to the vitamin A in pork liver, average and the standard deviation of each method measurement result are as follows:
| Method | (μ g.100g for vitamin A content -1） | Average recovery rate (%) |
| 1, saponification degrease method | 4638.2±302.3 | 95 |
| 2, anhydrous sodium sulfate anhydrates method | 4606.6±502.8 | 93 |
| 3, the method for the embodiment of the present invention 1 | 4680.7±125.6 | 97 |
It is little that result shows difference between method of the present invention 5 measurement results, and extraction ratio is high, and result is more accurate.
embodiment 2
1, sample freeze drying: get 1mL milk sample and be placed in 15mL test tube, freeze drying 2 hours, makes the residual moisture content in sample be less than 2%.
2, chloroform alcohol is extracted:
1) sample after freeze drying is added 3mL chloroform alcohol mixed liquor (chloroform: ethanol=2:1).
2) lucifuge lixiviate is after 2 hours, adds 1mL physiological saline, with vortex mixer 2800 turns/min, shakes 30 seconds.
Refrigerated centrifuge 4 DEG C, 3000 turns/min, centrifugal 5min.
3) take off layer chloroform extracted solution to add in another clean 10mL test tube.
4) in remaining sample residue, add 3mL chloroform alcohol mixed liquor again repeat to extract once, extracted twice liquid is merged.
3, ethanol redissolution purifying:
1) test tube containing above-mentioned merging extract is placed in 26 DEG C of water-baths, dries up with nitrogen.
2) in the test tube dried up, add 1.5mL ethanol, with vortex mixer 1500 turns/min, shake 30 seconds, redissolve and purification of vitamin A.
3) move in another test tube by this vitamin A alcohol solution, under same 26 DEG C of water bath condition, nitrogen dries up.
4, upper machine testing:
1) above-mentioned test tube is added 500 μ L ethanol, with vortex mixer 1500 turns/min, shake 30 seconds, and with ultrasonic echography 30 second, vitamin A is fully dissolved.
2) machine testing on 20 μ l is got.
Result
Adopt the three kinds of methods mentioned in literary composition respectively to carry out extraction and analysis 5 times to the vitamin A in milk, average and the standard deviation of each method measurement result are as follows:
| Method | (μ g.100g for vitamin A content -1） | Average recovery rate (%) |
| 1, saponification degrease method | 20.6 ± 3.0 | 94 |
| 2, anhydrous sodium sulfate anhydrates method | 21.9 ± 4.3 | 91 |
| 3, the method for the embodiment of the present invention 2 | 22.0 ± 1.2 | 96 |
It is little that result shows difference between method of the present invention 5 measurement results, and extraction ratio is high, and result is more accurate.
Claims (2)
1. in food, vitamin A detects the extraction process method analyzed, and comprises following processing step:
Step 1: sample freeze drying: get appropriate foodstuff samples freeze drying 2-10 hour, make the residual moisture content in sample be less than 2%;
Step 2: chloroform alcohol is extracted:
1) add the chloroform alcohol mixed liquor of 10-30 times of volume in the sample after freeze drying, described chloroform alcohol mixed liquor is that chloroform and ethanol mix according to volume ratio 2:1;
2) sample is smashed homogenate completely and lucifuge lixiviate 2 hours, add physiological saline, with vortex mixer 2800 turns/min, shake 30 seconds, the protein denaturation in sample solution is separated out;
3), after concussion mixing, 4 DEG C, 3000 turns/min, centrifugal 5min, collects lower floor's chloroform extracted solution; Again repeat to extract once to remaining sample residue with described chloroform alcohol mixed liquor, extracted twice liquid is merged;
Step 3: ethanol redissolution purifying:
1) test tube will be placed in containing above-mentioned merging extract, under 26 DEG C of water bath condition, dry up with nitrogen;
2) in the test tube dried up, add ethanol in proper amount, with vortex mixer 1500 turns/min, shake 30 seconds, obtain ethanol extract;
3) above-mentioned ethanol extract is moved to another test tube, after drying up with nitrogen, again add ethanol in proper amount redissolution purifying;
4) machine testing on ethanol in proper amount redissolution liquid is got.
2. in food according to claim 1, vitamin A detects the extraction process method analyzed, when it is characterized in that in step 1, foodstuff samples is solid, first foodstuff samples cleans, and dries, and cutting into thickness is that the sheet bulk of 0.3-0.5cm carries out freeze drying again.
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| CN201410123455.2A CN103852367B (en) | 2014-03-31 | 2014-03-31 | In a kind of food, vitamin A detects the extraction process method analyzed |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3035981A (en) * | 1958-10-20 | 1962-05-22 | Collett Week Corp | Process for extracting vitamin a from source oils |
| CN101393177A (en) * | 2008-10-13 | 2009-03-25 | 杭州民生药业集团有限公司 | Vitamin A content detection method by high performance liquid chromatography |
| CN102253130A (en) * | 2010-12-24 | 2011-11-23 | 天津天狮生物发展有限公司 | Method for measuring vitamins A, D and E in compound vitamin |
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2014
- 2014-03-31 CN CN201410123455.2A patent/CN103852367B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3035981A (en) * | 1958-10-20 | 1962-05-22 | Collett Week Corp | Process for extracting vitamin a from source oils |
| CN101393177A (en) * | 2008-10-13 | 2009-03-25 | 杭州民生药业集团有限公司 | Vitamin A content detection method by high performance liquid chromatography |
| CN102253130A (en) * | 2010-12-24 | 2011-11-23 | 天津天狮生物发展有限公司 | Method for measuring vitamins A, D and E in compound vitamin |
Non-Patent Citations (2)
| Title |
|---|
| 测定食品中维生素A的两种方法比较;覃章贵等;《粮食储藏》;19891231;第18卷;23-29，13 * |
| 高效液相色谱色谱法测定牛奶及乳制品中维生素A的研究分析;方景泉等;《中国新技术新产品》;20131231(第01期);1 * |
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Inventor after: Li Lei Inventor after: Su Yanwen Inventor after: Li Yuqing Inventor after: Chen Xiaoxuan Inventor after: Jiang Lingling Inventor after: Zhong Jinyi Inventor before: Li Lei Inventor before: Su Yanwen Inventor before: Chen Xiaoxuan Inventor before: Jiang Lingling Inventor before: Zhong Jinyi |
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