CN103852367A - Extracting processing method for detecting and analyzing vitamin A in food - Google Patents
Extracting processing method for detecting and analyzing vitamin A in food Download PDFInfo
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- CN103852367A CN103852367A CN201410123455.2A CN201410123455A CN103852367A CN 103852367 A CN103852367 A CN 103852367A CN 201410123455 A CN201410123455 A CN 201410123455A CN 103852367 A CN103852367 A CN 103852367A
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Abstract
The invention belongs to the field of fine chemical engineering extraction, and particularly relates to an extracting processing method for detecting and analyzing vitamin A in food. The extracting processing method comprises the following steps of firstly, carrying out freeze drying on a food sample to remove moisture, adding the food sample after freeze drying in a chloroform and ethyl alcohol mixed solution and carrying out high-speed homogenate, centrifuging a homogenate sample, collecting a chloroform extracting solution positioned on the lower layer, drying the extracting solution by using nitrogen, and adding ethyl alcohol to redissolve and purify vitamin A, wherein ultrasonic wave hydrotropy is adopted in the redissolving step so that the dissolved vitamin A is fully extracted. The extracting processing method provided by the invention has the characteristics that processes such as an alkali liquor saponification degreasing process and a reduced-pressure distillation process in a traditional method are not needed, the problems that the food sample is incompletely dehydrated and the like caused by water absorption when anhydrous sodium sulfate is added for grinding are solved, the operation is convenient, the time is shortened, the extraction efficiency is high and the like, the dangerousness caused by application of diethyl ether or normal hexane or methyl alcohol to extraction of a solvent is also overcome, and the result is not influenced even if micro water content exists in the extracted sample because of the water solubility of ethyl alcohol.
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 of analyzing.
Background technology
Vitamin A is rich content in the foods such as animal's liver, fish-egg, full milk, cream, birds, beasts and eggs, with the highest in beef liver, sheep liver, is conventionally dissolved in the lipid material of food.In plant, do not contain established vitamin A, but contain 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, select suitable solvent and method that it is extracted and separated from food lipid material, it is the key link of determination and analysis vitamin A, moisture in food also can affect and extract fully contacting of solvent and lipid material, separate thereby hinder the extraction of vitamin A from lipid material, therefore in food, Fat and moisture is the key factor that affects vitamin A extraction efficiency.
In at present detecting food in vitamin A method, first foodstuff samples to be added appropriate alkaline liquor to carry out saponification processing, fat in sample is combined with alkali form saponified, and through washing except soap and remove lipid material, then the vitamin A in non-saponification sample is extracted with ether.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, after drying up remaining ether with nitrogen again, obtain vitamin A extract, finally with ethanol, vitamin A extract is dissolved and purified and upper machine testing.This method needs first foodstuff samples to be carried out to saponification processing, extract with ether again, also need ether extracted liquid to carry out processed and dissolve purification with ethanol, have leaching process complexity, used time is longer, easily causes many deficiencies such as the Oxidative demage of vitamin A.
For fear of the adverse effect of saponification process, also there is method to omit the process of saponification, adopt adding anhydrous sodium sulfate in sample, grind to absorb the moisture in sample at mortar, then repeatedly extract with ether or normal hexane.Extract, after nitrogen dries up, then is dissolved to purifying vitamin A upper machine testing with methyl alcohol.Although this kind of method omitted saponification process, exist the moisture removal in sample incomplete, and can therefore 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 to adopt ether or normal hexane or methyl alcohol as extracting solvent, it is large, volatile that solvent toxicity is extracted in existence, easily human body produced 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 of analyzing.
Technical scheme of the present invention is:
In food, vitamin A detects an extraction process method of analyzing, 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) in the sample after freeze drying, add the chloroform alcohol mixed liquor of 10-30 times of volume, described chloroform alcohol mixed liquor is that chloroform and ethanol mix according to volume ratio 2:1;
2) sample is smashed completely to homogenate lucifuge lixiviate 2 hours, added physiological saline, with turn/min of vortex mixer 2800, shake 30 seconds, the protein denaturation in sample solution is separated out;
3) after concussion mixes, 4 ℃, 3000 turn/min, centrifugal 5min, collects lower floor's chloroform extracted solution; Again with described chloroform alcohol mixed liquor, remaining sample residue is repeated to extract once, extracted twice liquid is merged;
Step 3: ethanol redissolution purifying:
1) will contain above-mentioned merging extract and be placed in test tube, under 26 ℃ of water bath condition, dry up with nitrogen;
2) in the test tube drying up, add appropriate ethanol, with turn/min of vortex mixer 1500, shake 30 seconds;
3) above-mentioned ethanol extract is moved to another test tube, after drying up with nitrogen, again add appropriate ethanol redissolution purifying;
4) get machine testing on appropriate ethanol redissolution liquid.
On the basis of above scheme, when in step 1, foodstuff samples is solid, first foodstuff samples cleans, and dries, and the sheet bulk that cuts into thickness and be 0.3-0.5cm is carried 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 of analyzing, and its technological process mainly comprises sample freeze drying, and chloroform alcohol is extracted, ethanol redissolution purifying.First the present invention carries out foodstuff samples freeze drying to remove moisture, again cryodesiccated foodstuff samples is added to chloroform alcohol mixed liquor high-speed homogenization, again by centrifugal homogenate sample and collect the chloroform extracted solution that is positioned at lower floor, after drying up extract with nitrogen, add ethanol to make vitamin A redissolution purifying, in redissolution step, adopt ultrasound wave hydrotropy, extract completely so that vitamin A dissolves.Extraction of the present invention does not need the process such as alkali lye saponification degrease and decompression distillation in classic method, also overcome and added anhydrous sodium sulfate to grind the problems such as the existing foodstuff samples of water suction dewaters not exclusively, there is easy and simple to handle, time shorten, extraction efficiency high, also having overcome application ether or normal hexane or methyl alcohol is the danger of extracting solvent.Water-soluble due to ethanol, even if thereby extract in sample and have minor amount of water, also can not exert an influence to result.
Embodiment
The specific embodiment of the present invention is as follows:
Embodiment 1:
1, clean cutting and grinding: take tap water and clean the pork liver 100mg drying 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) in the sample after freeze drying, add 3mL chloroform alcohol mixed liquor (chloroform: ethanol=2:1).
2), with turn/min of high-speed homogenization machine 8000, homogenate 2 min, smash pork liver completely and fully mix with solvent.After lucifuge lixiviate 2 hours, add 1mL physiological saline, with turn/min of vortex mixer 2800, shake 30 seconds.
3) after concussion mixes, 4 ℃ of refrigerated centrifuges, 3000 turn/min, centrifugal 5min, takes off layer chloroform extracted solution and adds in another clean 10mL test tube.
4) in remaining sample residue, add again 3mL chloroform alcohol mixed liquor to repeat to extract once, extracted twice liquid is merged.
3, ethanol redissolution purifying:
1) test tube that contains above-mentioned merging extract is placed in to 26 ℃ of water-baths, dries up with nitrogen.
2) in the test tube drying up, add 1.5mL ethanol, with turn/min of vortex mixer 1500, shake redissolve and purifying vitamin A 30 seconds.
4, upper machine testing:
This vitamin A ethanolic solution is moved in another test tube, and under same 26 ℃ of water bath condition, nitrogen dries up.The above-mentioned test tube that dries up is added to 500 μ L ethanol, with turn/min of vortex mixer 1500, shake 30 seconds, and with 30 seconds of ultrasonic echography, vitamin A is fully dissolved; Get machine testing on 20 μ l.
Adopt three kinds of methods mentioning 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, the anhydrous sodium sulfate method of anhydrating | 4606.6±502.8 | 93 |
| 3, the method for the embodiment of the present invention 1 | 4680.7±125.6 | 97 |
Result shows that between 5 measurement results of method of the present invention, difference is little, 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 to 3mL chloroform alcohol mixed liquor (chloroform: ethanol=2:1).
2) lucifuge lixiviate, after 2 hours, adds 1mL physiological saline, with turn/min of vortex mixer 2800, shakes 30 seconds.
4 ℃ of refrigerated centrifuges, 3000 turn/min, centrifugal 5min.
3) taking off layer chloroform extracted solution adds in another clean 10mL test tube.
4) in remaining sample residue, add again 3mL chloroform alcohol mixed liquor to repeat to extract once, extracted twice liquid is merged.
3, ethanol redissolution purifying:
1) test tube that contains above-mentioned merging extract is placed in to 26 ℃ of water-baths, dries up with nitrogen.
2) in the test tube drying up, add 1.5mL ethanol, with turn/min of vortex mixer 1500, shake redissolve and purifying vitamin A 30 seconds.
3) this vitamin A ethanolic solution is moved in another test tube, under same 26 ℃ of water bath condition, nitrogen dries up.
4, upper machine testing:
1) above-mentioned test tube is added to 500 μ L ethanol, with turn/min of vortex mixer 1500, shake 30 seconds, and with 30 seconds of ultrasonic echography, vitamin A is fully dissolved.
2) get machine testing on 20 μ l.
Result
Adopt three kinds of methods mentioning 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, the anhydrous sodium sulfate method of anhydrating | 21.9 ± 4.3 | 91 |
| 3, the method for the embodiment of the present invention 2 | 22.0 ± 1.2 | 96 |
Result shows that between 5 measurement results of method of the present invention, difference is little, and extraction ratio is high, and result is more accurate.
Claims (2)
1. in food, vitamin A detects an extraction process method of analyzing, 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) in the sample after freeze drying, add the chloroform alcohol mixed liquor of 10-30 times of volume, described chloroform alcohol mixed liquor is that chloroform and ethanol mix according to volume ratio 2:1;
2) sample is smashed completely to homogenate lucifuge lixiviate 2 hours, added physiological saline, with turn/min of vortex mixer 2800, shake 30 seconds, the protein denaturation in sample solution is separated out;
3) after concussion mixes, 4 ℃, 3000 turn/min, centrifugal 5min, collects lower floor's chloroform extracted solution; Again with described chloroform alcohol mixed liquor, remaining sample residue is repeated to extract once, extracted twice liquid is merged;
Step 3: ethanol redissolution purifying:
To contain above-mentioned merging extract and be placed in test tube, under 26 ℃ of water bath condition, dry up with nitrogen;
In the test tube drying up, add appropriate ethanol, with turn/min of vortex mixer 1500, shake 30 seconds;
Above-mentioned ethanol extract is moved to another test tube, after drying up with nitrogen, again add appropriate ethanol redissolution purifying;
Get machine testing on appropriate ethanol redissolution liquid.
2. in food according to claim 1, vitamin A detects the extraction process method of analyzing, while it is characterized in that in step 1, foodstuff samples is solid, first foodstuff samples cleans, and dries, and the sheet bulk that cuts into thickness and be 0.3-0.5cm is carried 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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| 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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| CN103852367B CN103852367B (en) | 2016-03-09 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114230501A (en) * | 2021-12-24 | 2022-03-25 | 河南省奥林特药业有限公司 | Preparation method of pork liver extract rich in vitamin A |
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 |
-
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 |
|---|
| 方景泉等: "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", 《中国新技术新产品》 * |
| 覃章贵等: "测定食品中维生素A的两种方法比较", 《粮食储藏》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114230501A (en) * | 2021-12-24 | 2022-03-25 | 河南省奥林特药业有限公司 | Preparation method of pork liver extract rich in vitamin A |
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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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