CN106841138B - A kind of method of inorganic selenium and organic selenium content in measurement Se-enriched yeast - Google Patents
A kind of method of inorganic selenium and organic selenium content in measurement Se-enriched yeast Download PDFInfo
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Abstract
The invention discloses a kind of methods of the content of inorganic selenium in measurement Se-enriched yeast, comprising the following steps: (1) weighs Se-enriched yeast, strong base solution is added into Se-enriched yeast, ultrasound dissolves Se-enriched yeast, then carry out heating water bath；Wherein, the ratio of the amount of the substance of hydroxide ion is 1g:15~35mmol in the quality of the Se-enriched yeast and strong base solution；(2) it after having heated, is cooled down, then is centrifuged, take supernatant；(3) acidity of supernatant obtained by regulating step (2) to pH value is 4~5, filters after standing, obtains filtrate；(4) 6~12mol/L aqueous hydrochloric acid solution is added into filtrate obtained by step (3), is diluted after boiling, the Se content in dilution acquired solution is measured using atomic fluorescence spectrophotometer.The method of measurement inorganic selenium of the present invention is easy to operate, and precision is high, and the rate of recovery is good.
Description
Technical field
The present invention relates to organic seleniums and inorganic in a kind of method for measuring Se content more particularly to a kind of measurement Se-enriched yeast
The method of Se content.
Background technique
Selenium has the different physiological roles such as anti-oxidant, antitumor, is one of important nutrient of animal, is widely used in feeding
In feed additives, the main addition form of selenium has inorganic sodium selenite salt and organic selenium yeast, sodium selenite toxicity is high, be not easy by
Animal is absorbed and utilized, and easily causes waste and environmental pollution, and current most of areas have been prohibited from using, and selenium yeast is due to its generation
Thank to the features such as period is long, and bioavailability is high, and toxicity is low.Mainly with selenoprotein, nucleic acid, greasiness existing for-divalent in selenium yeast
The organic selenium of class and a small amount of sodium selenite, sodium selenate.Therefore, the content for detecting inorganic selenium and organic selenium in selenium yeast, is being raised
It is of great significance in material safe handling.
Currently, selenium yeast, as a kind of important feed additive, the measuring method of total selenium mainly has benzidine ultraviolet
Spectrophotometry, atomic fluorescence spectrum, inductively coupled plasma method, wherein hydride generation atomic fluorescence photometry has been introduced into
In national standard Law；For the measuring method of organic selenium there is presently no sole criterion, reporting more mainly has mass spectrum-efficient liquid phase
Chromatography, derivative-high performance liquid chromatography, ICP-MS (Rajani Jagtap, 2016) or HPLC-HG-AFS (Wang Jinrong,
2013) etc., but these methods are higher to instrument requirements, and expensive reagents, common laboratory is difficult to realize, cumbersome, test week
Phase is longer, and higher cost is not suitable for being widely popularized, in addition, there are also certain methods using the extraction of organic buffer solution, dialysis point
From method measure organic selenium (Gao Jianzhong, 2006), but this method takes a long time.
Summary of the invention
It is short, simple and be easy to it is an object of the invention to provide a kind of minute in place of overcome the deficiencies in the prior art
The method of inorganic Se content in the measurement Se-enriched yeast of implementation.
Another object of the present invention is to provide a kind of methods of organic selenium content in measurement Se-enriched yeast.
To achieve the above object, the technical solution used in the present invention are as follows:
A kind of method of the content of inorganic selenium in measurement Se-enriched yeast, comprising the following steps:
(1) Se-enriched yeast is weighed, strong base solution is added into Se-enriched yeast, ultrasound dissolves Se-enriched yeast, then carry out water
Bath heating；Wherein, in the quality of the Se-enriched yeast and strong base solution the ratio of the amount of the substance of hydroxide ion be 1g:15~
35mmol (i.e. according to the ratio that 15~35mmol strong base solution is added in every gram of Se-enriched yeast, highly basic is added into Se-enriched yeast
Solution；Wherein, in strong base solution the substance of highly basic amount by the substance of hydroxide ion in highly basic meter)；
(2) it after having heated, is cooled down, then is centrifuged, take supernatant；
(3) acidity of supernatant obtained by regulating step (2) is filtered after standing, is filtered until the pH value of supernatant is 4~5
Liquid；
(4) aqueous hydrochloric acid solution of 6~12mol/L is added into filtrate obtained by step (3), is diluted after boiling, uses
The content of inorganic selenium in atomic fluorescence spectrophotometer measurement dilution acquired solution.
Preferred embodiment as the method for the content of inorganic selenium in measurement Se-enriched yeast of the present invention, wherein In
In the step (1), the strong base solution is at least one of sodium hydroxide solution, potassium hydroxide solution.It is highly preferred that institute
Stating strong base solution is sodium hydroxide solution.It is highly preferred that the concentration of the sodium hydrate aqueous solution is 0.15~0.35mol/L,
It is highly preferred that the concentration of the sodium hydrate aqueous solution is 0.25mol/L.It is worth noting that, the concentration of sodium hydroxide is to selenium
The extraction effect of inorganic selenium is affected in yeast, and by largely testing, inventor's discovery is dense when sodium hydrate aqueous solution
Degree can obtain ideal extraction effect in the range of 0.15~0.35mol/L.
Preferred embodiment as the method for the content of inorganic selenium in measurement Se-enriched yeast of the present invention, wherein In
In the step (1), the bath temperature be 45~65 DEG C, when bath temperature in the range when, for nothing in Se-enriched yeast
The extraction effect of machine selenium influences smaller.It is further preferable that the bath temperature is 65 DEG C.
In the step (1), water bath time depends on bath temperature, in selectable range (i.e. 45~65 DEG C),
When temperature is relatively high, water bath time is relatively short, on the contrary.But when water bath time is more than 30 minutes, for Se-enriched yeast
The effect that middle inorganic selenium extracts is not significantly improved.
Preferred embodiment as the method for the content of inorganic selenium in measurement Se-enriched yeast of the present invention, wherein In
In the step (3), the pH of supernatant is adjusted to 4.5, this is because pH=4.5 is the isoelectric point of protein in Se-enriched yeast,
At the pH, the solubility of protein is minimum in Se-enriched yeast.It is further preferable that the pH of supernatant is adjusted to 4.5 with hydrochloric acid, from
And excessive substance is avoided to be introduced into solution to be detected.
Preferred embodiment as the method for the content of inorganic selenium in measurement Se-enriched yeast of the present invention, wherein former
The running parameter of sub- fluophotometer is arranged are as follows: instrument work negative high voltage: 280V, hollow cathode lamp current: 80mA, carrier gas stream
Amount: 400mL/min, shield gas flow amount: 900mL/min, atomizing furnace height: 8mm, the reading duration: 15s, delay time: 3s,
Carrier fluid: 5%HCl (mass percent concentration), reducing agent: 2%KBH4+ 0.5%NaOH.
It is worth noting that, the content of+4 valence selenium can only be measured in atom fluorescent luminosity principle, there is+6 in Se-enriched yeast,
+ 4, three kinds of Se forms of-divalent, wherein it is organic selenium (a large amount of selenoproteins, a small amount of nucleic acid) that-divalent is existing ,+6 ,+4 valences are solvable
Property inorganic selenium salt (selenate, selenite), in the step (1), in the sample of Se-enriched yeast be added strong base solution (ratio
Such as, sodium hydrate aqueous solution, potassium hydroxide aqueous solution), it can effectively change Se-enriched yeast cell wall structure at a certain temperature,
Enhance permeability, to improve the extraction effect of inorganic selenium in Se-enriched yeast.In addition, in the step (3), by by pH tune
The isoelectric point of protein into Se-enriched yeast can remove the soluble selenium albumen in extracting solution, to avoid-right+4 valence of divalent selenium
The interference (the having faint interference of right+4 valence Determination of Selenium of-divalent selenium) of Determination of Selenium.In addition, in the step (5),
Under conditions of hydrochloric acid is added and heats ,+6 valence selenium in the sample of Se-enriched yeast can be reduced to+4 valences, to pass through hydride
AFS DETERMINATION goes out inorganic Se content.
In addition, technical solution is such as the invention also discloses a kind of method of the content of organic selenium in measurement Se-enriched yeast
Under:
A kind of method of the content of organic selenium in measurement Se-enriched yeast, comprising the following steps:
(a) content of total selenium in Se-enriched yeast is measured；
(b) content of inorganic selenium in Se-enriched yeast is measured according to the above method；
(c) it calculates organic selenium content in selenium yeast: calculating organic selenium content in Se-enriched yeast: the selenium that step (a) is measured
Total Se content subtracts inorganic Se content in the Se-enriched yeast that step (b) measures in yeast, and resulting difference is in Se-enriched yeast
Organic selenium content.
Wherein, in the step (a), measurement for total Se content can use measuring method known in the art.
As the preferred embodiment of the method for the content of organic selenium in measurement Se-enriched yeast of the present invention, the side of total Se content is measured
Method be GB/T13883-2008 " measurement of selenium in feed " in record " Hydride generation fluorescence spectrometry is (that is, HG-AFS
Method) ", the specific steps are as follows:
(1) Se-enriched yeast is weighed, according to the ratio that 7.5mL mixed acid is added in every gram of Se-enriched yeast, into Se-enriched yeast
Mixed acid is added, digestion is overnight；Wherein, the mixed acid is made of nitric acid and perchloric acid, the volume of the nitric acid and perchloric acid
Than for 4:1；
(2) the resulting solution of hot digestion, until perchloric acid smoked in solution；
(3) cooling, 2.5mL hydrochloric acid is added, continues to be heated to perchloric acid smoked, it is cooling；
(4) acquired solution after step (3) cooling is moved into 50mL volumetric flask, constant volume；
(5) it takes 20mL step (4) acquired solution into 50mL volumetric flask, 8mL hydrochloric acid is added and 2mL concentration is 200g/L's
Potassium ferricyanide solution is diluted with water to scale, obtains sample solution, then using total selenium in atomic fluorescence spectrophotometer measurement sample solution
Content.
Compared with prior art, technical solution of the present invention has the advantages that
1, the method for inorganic Se content passes through alkali thermal method (for example, using sodium hydroxide in measurement selenium yeast of the present invention
The method of heating extraction) recovery rate of inorganic selenium is improved, and organic selenium pair is reduced by adjusting pH to isoelectric points of proteins
In the interference of inorganic Determination of Selenium, to improve the accuracy of inorganic Determination of Selenium.
2, the present invention uses general acid-base reagent and common instrument, can be achieved in Se-enriched yeast in common laboratory
The measurement of inorganic selenium and organic selenium content；In addition, the present invention extracts selenium-rich ferment using strong base solution (for example, sodium hydroxide solution)
The restricted-access media speed of inorganic selenium is fast in mother, and the used time is short, and minute process is no more than 1 hour.
3, the method for inorganic selenium is easy to operate in measurement Se-enriched yeast of the present invention, and precision is high, and the rate of recovery is good, In
Under optimal conditions, the detection of inorganic selenium is limited to 0.0201 μ g/L, and the range of linearity is 0~40 μ g/L, passes through recovery testu, nothing
Machine selenium recovery is 79.6%~85.9%.
4, the method for organic selenium content passes through HG-AFS (hydride generation-original in measurement Se-enriched yeast of the present invention
Sub- fluorescence spectrum) content of total selenium, inorganic selenium in method measurement Se-enriched yeast, in conjunction with minusing (that is, organic selenium content=total selenium
The inorganic Se content of content -) organic selenium content is calculated, so that the step of simplifying organic selenium content measurement, shortens minute.
Detailed description of the invention:
Fig. 1 is the standard curve that inorganic selenium standard solution obtains in present invention measurement Se-enriched yeast；
Fig. 2 is effect tendency figure of the naoh concentration to inorganic selenium extracted amount.
Specific embodiment
To better illustrate the object, technical solutions and advantages of the present invention, the present invention is made combined with specific embodiments below
It further illustrates.
In following embodiments, used materials and methods are as follows:
Material and reagent: potassium borohydride, concentrated hydrochloric acid, concentrated nitric acid, perchloric acid (be excellent pure grade, i.e., it is commercially available not diluted
Acid), high purity water, selenium standard solution (State center for standard matter).Mixed acid: nitric acid: perchloric acid=4: 1 (stoste volume ratio,
Total Determination of Selenium resolution is used), solution of potassium borohydride (atomic fluorescence spectrophotometer instrument reaction solution): weigh 1g sodium hydroxide
Add 200mL water to dissolve it sufficiently, adds 4g potassium borohydride and be uniformly mixed, now match and first use.
Instrument and AFS-2000 atomic fluorescence spectrophotometer (Beijing Kechuang sea light Co., Ltd), digital display constant temperature bath
(Shanghai Shen Sheng Bioisystech Co., Ltd), ultrasonic cleaner (Shanghai High Kudos Science Instrument Co., Ltd.), thermostatic electrothermal plate
(Lab-TechEH20B), low speed centrifuge (Jintan letter section instrument HDL-4).
In embodiment, atomic fluorescence spectrophotometer best operating condition: instrument work negative high voltage: 280V, hollow cathode lamp electricity
Stream: 80mA, carrier gas flux: 400mL/min, shield gas flow amount: 900mL/min, atomizing furnace height: 8mm, the reading duration:
15s, delay time: 3s, carrier fluid: 5%HCl (mass percent concentration), reducing agent: 2%KBH4+ 0.5%NaOH (1g hydroxide
Sodium adds 200mL water to dissolve it sufficiently, adds aqueous solution obtained from 4g potassium borohydride is uniformly mixed).
Instrument precision and detection limit: according to the optimum condition of instrument, the optimum linear range of linearity of selenium is 0~40 μ g/
Selenium standard solution (State center for standard matter) is diluted to 0 μ g/L, 10 μ g/L, 20 μ g/L, 40 μ g/L by L, and hydrochloric acid constant volume is pressed
According to the standard curve (referring to Fig. 1) of above operating condition measurement Se content, coefficient R2=0.9999 by 10 μ g/L
Standard selenium measures 5 times, obtains RSD=2.8%, this method has preferable precision.Meanwhile 11 groups of blank are measured, by 3
It is 0.0201 μ g/L that times standard deviation, which obtains detection limit (3 δ),.
The test of 1 accuracy of table
The measurement of the content of inorganic selenium in Se-enriched yeast:
(1) sodium hydrate aqueous solution containing 15~35mmol sodium hydroxide is added in every 1g Se-enriched yeast, passes through ultrasound
Dissolve Se-enriched yeast sufficiently；
(2) under conditions of temperature is 45~65 DEG C, at least water-bath cools down rapidly after 30 minutes；
(3) it is centrifuged, takes supernatant, with hydrochloric acid tune pH to 4.5 and stand at least 5 minutes；
(4) after filtering mixed liquor obtained by step (3) with filter paper, filtrate is taken, concentrated hydrochloric acid is added thereto, is boiled 2 minutes；
(5) mixed liquor obtained by step (4) is diluted with water to suitable concentration, inorganic selenium is measured using atomic fluorescence spectrophotometer
Content.
Embodiment 1
(1) sodium hydrate aqueous solution of 10mL 0.25mol/L is added in 0.1g Se-enriched yeast, selenium-rich is made by ultrasound
Yeast sufficiently dissolves；
(2) under conditions of temperature is 65 DEG C, water-bath cools down rapidly after 30 minutes；
(3) 4000r/min is centrifuged 10 minutes, takes supernatant, with the hydrochloric acid tune pH to 4.5 of 1mol/L and stands 5 minutes；
(4) after filtering mixed liquor obtained by step (3) with filter paper, filtrate is taken, 5mL concentrated hydrochloric acid is added thereto, boils 2 points
Clock；
(5) mixed liquor obtained by step (4) is diluted with water to suitable concentration, inorganic selenium is measured using atomic fluorescence spectrophotometer
Content.
Embodiment 2
(1) sodium hydrate aqueous solution of 10mL 0.25mol/L is added in 0.1g Se-enriched yeast, selenium-rich is made by ultrasound
Yeast sufficiently dissolves；
(2) under conditions of temperature is 45 DEG C, water-bath cools down rapidly after 30 minutes；
(3) 4000r/min is centrifuged 10 minutes, takes supernatant, with the hydrochloric acid tune pH to 4.5 of 1mol/L and stands 5 minutes；
(4) after filtering mixed liquor obtained by step (3) with filter paper, filtrate is taken, 5mL concentrated hydrochloric acid is added thereto, boils 2 points
Clock；
(5) mixed liquor obtained by step (4) is diluted with water to suitable concentration, inorganic selenium is measured using atomic fluorescence spectrophotometer
Content.
Embodiment 3
(1) sodium hydrate aqueous solution of 10mL 0.25mol/L is added in 0.1g Se-enriched yeast, selenium-rich is made by ultrasound
Yeast sufficiently dissolves；
(2) under conditions of temperature is 50 DEG C, water-bath cools down rapidly after 30 minutes；
(3) 4000r/min is centrifuged 10 minutes, takes supernatant, with the hydrochloric acid tune pH to 4.5 of 1mol/L and stands 5 minutes；
(4) after filtering mixed liquor obtained by step (3) with filter paper, filtrate is taken, 5mL concentrated hydrochloric acid is added thereto, boils 2 points
Clock；
(5) mixed liquor obtained by step (4) is diluted with water to suitable concentration, inorganic selenium is measured using atomic fluorescence spectrophotometer
Content.
Embodiment 4: influence of the sodium hydrate aqueous solution of various concentration to inorganic selenium extraction effect
5 parts of 0.1g Se-enriched yeast are accurately weighed, is placed in triangular flask, carries out inorganic Se content by step described in embodiment 1
Measurement, difference be only that in this 5 parts of samples be separately added into 0.15mol/L, 0.2mol/L, 0.25mol/L, 0.3mol/L,
The sodium hydrate aqueous solution 10mL of 0.35mol/L.
As shown in Fig. 2, naoh concentration is in 0.25mol/L, recovery rate highest.
Embodiment 5
(1) sodium hydrate aqueous solution of 10mL 0.25mol/L is added in 0.1g Se-enriched yeast, selenium-rich is made by ultrasound
Yeast sufficiently dissolves；
(2) under conditions of temperature is 65 DEG C, water-bath cools down rapidly after 30 minutes；
(3) 4000r/min is centrifuged 10 minutes, takes supernatant, with the hydrochloric acid tune pH to 4.0 of 1mol/L and stands 5 minutes；
(4) after filtering mixed liquor obtained by step (3) with filter paper, filtrate is taken, 5mL concentrated hydrochloric acid is added thereto, boils 2 points
Clock；
(5) mixed liquor obtained by step (4) is diluted with water to suitable concentration, inorganic selenium is measured using atomic fluorescence spectrophotometer
Content.
Embodiment 6
(1) sodium hydrate aqueous solution of 10mL 0.25mol/L is added in 0.1g Se-enriched yeast, selenium-rich is made by ultrasound
Yeast sufficiently dissolves；
(2) under conditions of temperature is 65 DEG C, water-bath cools down rapidly after 30 minutes；
(3) 4000r/min is centrifuged 10 minutes, takes supernatant, with the hydrochloric acid tune pH to 5.0 of 1mol/L and stands 5 minutes；
(4) after filtering mixed liquor obtained by step (3) with filter paper, filtrate is taken, 5mL concentrated hydrochloric acid is added thereto, boils 2 points
Clock；
(5) mixed liquor obtained by step (4) is diluted with water to suitable concentration, inorganic selenium is measured using atomic fluorescence spectrophotometer
Content.
Embodiment 7
(1) potassium hydroxide aqueous solution of 10mL 0.25mol/L is added in 0.1g Se-enriched yeast, selenium-rich is made by ultrasound
Yeast sufficiently dissolves；
(2) under conditions of temperature is 65 DEG C, water-bath cools down rapidly after 30 minutes；
(3) 4000r/min is centrifuged 10 minutes, takes supernatant, with the hydrochloric acid tune pH to 4.5 of 1mol/L and stands 5 minutes；
(4) after filtering mixed liquor obtained by step (3) with filter paper, filtrate is taken, the hydrochloric acid of 10mL6mol/L is added thereto
Aqueous solution boils 2 minutes；
(5) mixed liquor obtained by step (4) is diluted with water to suitable concentration, inorganic selenium is measured using atomic fluorescence spectrophotometer
Content.
Embodiment 8:
5 parts of Se-enriched yeast of the same race are taken respectively, and the measurement of inorganic Se content is carried out by the method for the present invention, is computed, the measurement
The relative standard deviation of method is 5.29% (as shown in table 2).
The measurement content of 2 inorganic selenium of table
Embodiment 9: inorganic selenium measurement result in sample
The commercially available Se-enriched yeast 0.1g of 3 kinds of differences is weighed respectively, and every kind of Se-enriched yeast takes 2 parts, respectively takes a and adds respectively
Enter 2.5 μ g, 5 μ g, 7.5 μ g inorganic seleniums (national standard solution selenium is obtained through dilution) are not added in remaining 3 parts, according to embodiment 2
The method measures the content of its inorganic selenium, as a result as shown in table 3 below.Wherein, the rate of recovery is calculated according to formula 1.
Formula 1:
Recovery of standard addition=(standardized sample measured value-blank sample measured value) scalar quantity × 100%. ÷
The measurement of the inorganic selenium recovery of table 3
When measuring the content of inorganic selenium in Se-enriched yeast sample it can be seen from upper table 3, method of the present invention is used
The rate of recovery with higher, this shows that method of the present invention is higher to the accuracy of measurement of inorganic selenium in Se-enriched yeast.
Embodiment 10
Total Determination of Selenium method:
By " Hydride atomic fluorescent spectrum method for detecting " recorded in GB/T13883-2008 " measurement of selenium in feed ", tool
Steps are as follows for body:
(1) Se-enriched yeast 2.0g is weighed, 0.0001g is accurate to, is placed in 100mL beaker, 15.0mL volume ratio, which is added, is
The nitric acid of 4:1 and the mixed solution of perchloric acid, digestion is overnight；
(2) next day heats on electric hot plate, when solution perchloric acid smoked, continues to be heated to liquor capacity to be 2mL or so,
It can't be evaporated；
(3) cooling, 2.5mL hydrochloric acid is added, purges surface plate and wall of cup with water, it is cold when continuing to be heated to perchloric acid smoked
But；
(4) step (3) acquired solution is moved into 50mL volumetric flask, is diluted with water to scale；
(5) it takes 20mL step (4) acquired solution to 50mL volumetric flask, the potassium ferricyanide of 8mL hydrochloric acid and 2mL200g/L is added
Solution is diluted with water to scale, then using the content of total selenium in atomic fluorescence spectrophotometer measurement dilution acquired solution.
Embodiment 11
Organic selenium content: pass through minusing, that is, the organic selenium content=inorganic Se content of total Se content-.
Embodiment 12
Analysis measurement is carried out to commercially available 3 kinds different Se-enriched yeasts using method of the present invention, as a result such as the following table 4 institute
Show.
The measurement of organic selenium and inorganic selenium in 4 Se-enriched yeast of table
According to " feed addictive safe handling specification " regulation, inorganic Se content must not exceed 2% in yeast selenium.By table 4
It is found that method according to the present invention is measured, commercially available 3 kinds of Se-enriched yeasts meet regulation.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than protects to the present invention
The limitation of range is protected, although the invention is described in detail with reference to the preferred embodiments, those skilled in the art should
Understand, it can be with modification or equivalent replacement of the technical solution of the present invention are made, without departing from the essence of technical solution of the present invention
And range.
Claims (8)
1. a kind of method of inorganic Se content in measurement Se-enriched yeast, it is characterised in that: the following steps are included:
(1) Se-enriched yeast is weighed, strong base solution is added into Se-enriched yeast, ultrasound dissolves Se-enriched yeast, then carry out water-bath and add
Heat；Wherein, in the quality of the Se-enriched yeast and strong base solution the ratio of the amount of the substance of hydroxide ion be 1g:15~
35mmol；The temperature of heating water bath is 45~65 DEG C, and the time of heating water bath is 30 minutes or more；
(2) it after having heated, is cooled down, then is centrifuged, take supernatant；
(3) acidity of supernatant obtained by regulating step (2) filters after standing until the pH value of supernatant is 4~5, obtains filtrate；
(4) 6~12mol/L aqueous hydrochloric acid solution is added into filtrate obtained by step (3), is diluted after boiling, it is glimmering using atom
Light photometric determination dilutes the content of the inorganic selenium in acquired solution.
2. measuring the method for inorganic Se content in Se-enriched yeast as described in claim 1, it is characterised in that: the strong base solution
For at least one of sodium hydroxide solution, potassium hydroxide solution.
3. measuring the method for inorganic Se content in Se-enriched yeast as claimed in claim 2, it is characterised in that: the strong base solution
For sodium hydroxide solution, the concentration of sodium hydroxide is 0.15~0.35mol/L in the sodium hydroxide solution.
4. measuring the method for inorganic Se content in Se-enriched yeast as claimed in claim 3, it is characterised in that: the sodium hydroxide
The concentration of sodium hydroxide is 0.25mol/L in solution.
5. measuring the method for inorganic Se content in Se-enriched yeast as described in claim 1, it is characterised in that: the step (1)
In, the temperature of heating water bath is 65 DEG C.
6. measuring the method for inorganic Se content in Se-enriched yeast as described in claim 1, it is characterised in that: the step (3)
In, the acidity of supernatant obtained by regulating step (2), until the pH value of supernatant is 4.5.
7. a kind of method of organic selenium content in measurement Se-enriched yeast, it is characterised in that: the following steps are included:
(a) total Se content in Se-enriched yeast is measured；
(b) using inorganic Se content in any one of claim 1~6 the method measurement Se-enriched yeast；
(c) it calculates organic selenium content in Se-enriched yeast: Se content total in selenium yeast that step (a) measures being subtracted into step (b) and is surveyed
Inorganic Se content in the Se-enriched yeast obtained, resulting difference is organic selenium content in Se-enriched yeast.
8. measuring the method for organic selenium content in Se-enriched yeast as claimed in claim 7, it is characterised in that: the step (a)
Are as follows:
(1) Se-enriched yeast is weighed, according to the ratio that 7.5mL mixed acid is added in every gram of Se-enriched yeast, is added into Se-enriched yeast
Mixed acid, digestion is overnight；Wherein, the mixed acid is made of nitric acid and perchloric acid, and the volume ratio of the nitric acid and perchloric acid is
4:1；
(2) the resulting solution of hot digestion, until perchloric acid smoked in solution；
(3) cooling, 2.5mL hydrochloric acid is added, continues to be heated to perchloric acid smoked, it is cooling；
(4) acquired solution after step (3) cooling is moved into 50mL volumetric flask, constant volume；
(5) it takes 20mL step (4) acquired solution into 50mL volumetric flask, 8mL hydrochloric acid and 2mL concentration is added as the iron cyanogen of 200g/L
Change potassium solution, be diluted with water to scale, obtains sample solution, then contain using total selenium in atomic fluorescence spectrophotometer measurement sample solution
Amount.
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| CN103217407A (en) * | 2013-04-18 | 2013-07-24 | 衢州市质量技术监督检测中心 | Content measuring method for organic selenium, protein selenium, polysaccharide selenium or RNA selenium in selenium-rich rice |
| CN103884785A (en) * | 2013-12-09 | 2014-06-25 | 恩施土家族苗族自治州农业科学院 | Selenium detection method |
| CN104101655A (en) * | 2013-04-11 | 2014-10-15 | 北京瑞利分析仪器有限公司 | Method for detection of content of selenate radicals and online reduction of selenate radicals to selenite radicals |
| CN104931468A (en) * | 2015-03-23 | 2015-09-23 | 浙江大学 | Method for determining content of total selenium, inorganic selenium and organic selenium of selenium yeast |
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| CN102550795A (en) * | 2011-12-26 | 2012-07-11 | 苏州硒谷科技有限公司 | Method for extracting selenium-containing protein from selenium-enriched yeast |
| US20160130144A1 (en) * | 2014-11-11 | 2016-05-12 | Gioulchen Tairova | Method and Process of Treatment of Selenium Containing Material and Selenium Recovery |
| CN105277636B (en) * | 2015-09-25 | 2017-10-27 | 中国科学技术大学苏州研究院 | Se form method for measuring in a kind of high selenium fungi |
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| CN104101655A (en) * | 2013-04-11 | 2014-10-15 | 北京瑞利分析仪器有限公司 | Method for detection of content of selenate radicals and online reduction of selenate radicals to selenite radicals |
| CN103217407A (en) * | 2013-04-18 | 2013-07-24 | 衢州市质量技术监督检测中心 | Content measuring method for organic selenium, protein selenium, polysaccharide selenium or RNA selenium in selenium-rich rice |
| CN103884785A (en) * | 2013-12-09 | 2014-06-25 | 恩施土家族苗族自治州农业科学院 | Selenium detection method |
| CN104931468A (en) * | 2015-03-23 | 2015-09-23 | 浙江大学 | Method for determining content of total selenium, inorganic selenium and organic selenium of selenium yeast |
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