CN103217407A - Content measuring method for organic selenium, protein selenium, polysaccharide selenium or RNA selenium in selenium-rich rice - Google Patents

Content measuring method for organic selenium, protein selenium, polysaccharide selenium or RNA selenium in selenium-rich rice Download PDF

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CN103217407A
CN103217407A CN2013101355603A CN201310135560A CN103217407A CN 103217407 A CN103217407 A CN 103217407A CN 2013101355603 A CN2013101355603 A CN 2013101355603A CN 201310135560 A CN201310135560 A CN 201310135560A CN 103217407 A CN103217407 A CN 103217407A
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selenium
rich rice
rna
polysaccharide
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祝华明
方建军
张旭
郑睿行
鲍利锋
龚鸿萍
方芳
夏爱萍
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QUZHOU QUALITY TECHNOLOGY SUPERVISION INSPECTION CENTER
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Abstract

The invention relates to a detecting method for selenium speciation analysis in selenium-rich rice and particularly relates to a detecting method for organic selenium, protein selenium, polysaccharide selenium or RNA selenium in selenium-rich rice. The measuring method comprises the following steps of: (1) preparing a sample, namely sealing and storing selenium-rich rice flour to be detected for future use, wherein organic selenium is extracted through a dialysis method, and protein selenium, polysaccharide selenium and RNA selenium are respectively extracted; (2) measuring the selenium content through hydride atomic fluorescence spectrometry under measuring conditions that the negative high pressure is 340V, the lamp current is 100mA, the atomization temperature is 800 DEG C, the furnace height is 8mm, the flow rate of carrier gas is 500mL/min, the flow rate of shielding gas is 1000mL/min, the delay time is 1 second, the reading time is 10 seconds, the liquid adding time is 8 seconds, and the sample feeding volume is 2mL; and (3) data processing. The detecting method disclosed by the invention has the advantages of high sensitivity and accuracy and simplicity in operation.

Description

Organic selenium, albumen selenium, polysaccharide selenium or RNA Se content assay method in the selenium-rich rice
Technical field
The present invention relates to the detection method of selenium morphological analysis in the selenium-rich rice, especially relate to the detection method of organic selenium in a kind of selenium-rich rice, albumen selenium, polysaccharide selenium or RNA selenium.
Background technology
Selenium is one of trace element essential among the human life activity, gets more and more people's extensive concerning in recent years.It has the flight against senium of human body of making, prevention canceration, protection and repairs different physiological roles such as vegetative cell, detoxication and toxicant eliminating function, raising immunity, is called as one of element of dominating life.Selenium is very clear and definite to the importance of human body, but authoritative data shows that the function of selenium is different and different with its form, the existence of inorganic selenium is harmful to human body in the food, the selenium of inorganic form particularly hexavalent selenium toxicity is very big, human body is had no nutrition can say to have only the selenium of organic form, as selenoprotein, seleno-amino acids, selenium polypeptide, selenium polysaccharide etc., in body, just can change physiological activator into, by human body is absorbed.
At present, actually rare about the research of Se-rich farm products and food both at home and abroad, detection to useful selenium form more relates to very few with analysis, therefore carry out useful selenium morphological analysis technical research in the Se-rich farm products very necessary, help people's rich selenium product of wise selection health rationally, the science meals have important practical significance.
Summary of the invention
The objective of the invention is to solve the difficult problem that the selenium morphological analysis detects in the Se-rich farm products, the detection method of organic selenium in a kind of selenium-rich rice, albumen selenium, polysaccharide selenium or RNA selenium is provided, that detection method of the present invention has is highly sensitive, accuracy good, advantage simple to operate.
The technical solution adopted for the present invention to solve the technical problems is:
Organic selenium, albumen selenium, polysaccharide selenium or RNA Se content assay method in the selenium-rich rice, described assay method comprises the following steps:
(1) preparation of sample: it is 100 purpose selenium-rich rice dry powder that selenium-rich rice to be detected is pulverized the acquisition granularity, and sealed storage is standby;
1. the extraction of organic selenium: take by weighing above-mentioned selenium-rich rice dry powder 1.00g, add 5 ~ 10ml ultrapure water, further grinding fully breaks selenium-rich rice dry powder, quantitatively be transferred in the bag filter, with the ultrapure water 24h that dialyses, dialyzed sample is taken out, and centrifugal 15min obtains precipitation under the 12000rpm condition, and described precipitation vacuum drying gets organic selenium m 1G;
2. the extraction of albumen selenium: take by weighing above-mentioned selenium-rich rice dry powder 10.00g, in the 500ml triangular flask, add 0.05mol/LNaOH solution 100ml vibration 2h and get mixed liquor, with mixed liquor centrifugal 15min under the 12000rpm condition, get supernatant, add 0.1mol/LHCl and regulate pH to 5.5, centrifugal 15min must precipitate under the 12000rpm condition once more, and described precipitation vacuum drying is got albumen selenium m 2G;
3. the extraction of polysaccharide selenium: take by weighing above-mentioned selenium-rich rice dry powder 2.00g, add 100ml 0.5mol/LNaOH solution, extract polysaccharide in 80 ℃ of water-bath heating 2h, centrifugal 15min under the 12000rpm condition gets supernatant and washs 3 times with chloroform-butanol solution then, to remove the floating preteins of crude polysaccharides, the volume ratio of described chloroform and normal butyl alcohol is 24:1, and adding absolute ethyl alcohol to the final concentration of alcohol of solution then is 80%, leaves standstill 24h, collecting precipitation gets polysaccharide selenium m with described precipitation vacuum drying 3G;
4. the extraction of RNA selenium: take by weighing above-mentioned selenium-rich rice dry powder 10.00g, add 200ml 0.025mol/LNaOH solution shake and swing 45min, transfer pH to 7.0 with 3mol/L hydrochloric acid then, be heated to 90 ℃ after stirring 10min, be cooled to 10 ℃ behind the insulation 10min, in the centrifugal 15min of 12000rpm, get supernatant and transfer pH to 2.5 with 6mol/L hydrochloric acid, 5 ℃ of refrigeration standing over night, once more in the centrifugal 15min of 12000rpm, collecting precipitation adds 1 ~ 2 ammoniacal liquor, use the 30ml dissolved in distilled water, wash 3 times with chloroform-butanol solution, the volume ratio of described chloroform and normal butyl alcohol is 24:1, and the water oven dry that obtains is obtained RNA selenium m 4G;
(2) Determination of Selenium Contents
1. typical curve: by the concentration gradient drawing standard curve of 0,4,8,12,16,20 μ g/L;
2. digestive juice preparation: take by weighing above-mentioned organic selenium, albumen selenium, polysaccharide selenium and RNA selenium 0.3g respectively in the 50ml triangular flask, add 10ml by HNO 3And HClO 4By volume 4:1 mixed acid mixture, cold digestion is spent the night, next day, hot digestion when solution becomes limpid colourlessly and when occurring with white cigarette, continued to be heated to about residual volume 2ml again, cooling, add 5ml 6mol/L hydrochloric acid again, continue to be heated to solution and become limpid colourless and cooling occurs with white cigarette, transfer is settled to 50ml, obtains digestive juice;
3. measure: get each 2ml of above-mentioned digestive juice respectively in the 10ml color comparison tube, add concentrated hydrochloric acid 2ml, add water and be settled to 10ml, adopt the hydride generation atomic fluorescence method to measure behind the mixing, obtain peak area fluorescent value X successively 1, X 2, X 3,X 4, with peak area fluorescent value X 1, X 2, X 3,X 4Bringing typical curve acquisition organic selenium, albumen selenium, polysaccharide selenium and RNA selenium digestive juice selenium concentration respectively into is Y 1, Y 2, Y 3, Y 4
(3) data processing
1. organic selenium content=Y in the selenium-rich rice 1* 0.25 ÷ 0.3* m 1÷ selenium-rich rice quality, wherein the selenium-rich rice quality is 1.00g;
2. albumen Se content=Y in the selenium-rich rice 2* 0.25 ÷ 0.3* m 2÷ selenium-rich rice quality, wherein the selenium-rich rice quality is 10.00g;
3. organic selenium content=Y in the selenium-rich rice 3* 0.25 ÷ 0.3* m 3÷ selenium-rich rice quality, wherein the selenium-rich rice quality is 2.00g;
4. organic selenium content=Y in the selenium-rich rice 4* 0.25 ÷ 0.3* m 4÷ selenium-rich rice quality, wherein the selenium-rich rice quality is 10.00g.
As preferably, the specification that organic selenium extracts the bag filter that adopts is 8000Da, ultrapure water of the centrifugal replacing of every 6h in the dialysis procedure.
As preferably, described vacuum drying vacuum tightness is-0.085 ~-0.095Mpa, vacuum drying temperature is 50 ~ 60 ℃.
As preferably, the mass concentration of used ammoniacal liquor was 25~28% during RNA selenium extracted.
As preferably, hydride generation atomic fluorescence method condition determination is: negative high voltage: 340 V; Lamp current: 100 mA; Atomization temperature: 800 ℃; Stove height: 8 mm; Flow rate of carrier gas 500 mL/min; Shield gas flow speed: 1 000mL/min; Time delay: 1 s; Reading duration: 10 s; The liquid feeding time: 8 s; Sampling volume: 2 mL.
The invention has the beneficial effects as follows: the present invention is by the extraction process of science reasonable in design, organic selenium, albumen selenium, polysaccharide selenium and RNA selenium in the selenium-rich rice are proposed out efficiently, measure by the hydride generation atomic fluorescence method then, have accuracy height, precision is good, the recovery is high advantage, reagent and equipment that assay method simultaneously of the present invention adopts all are conventional reagent and equipment, the detection cost is low, convenient enforcement.
Description of drawings
Fig. 1 is a selenium canonical plotting of the present invention.
Embodiment
Below by specific embodiment, and in conjunction with the accompanying drawings, technical scheme of the present invention is described in further detail.
Material: selenium-rich rice picks up from the rich selenium of Quzhou City, Zhejiang Province dragon trip county annals Chinese bush cherry area;
Reagent: nitric acid, hydrochloric acid, that perchloric acid is top grade is pure, and NaOH, absolute ethyl alcohol, chloroform, normal butyl alcohol, ammoniacal liquor, sodium borohydride are pure for analyzing, and the selenium standard solution disposes with reference to GB5009.93-2010;
Instrument and equipment: two pass atomic fluorescence spectrophotometer (AFS-930), electric hot plate (DB-2A), mortar, comminutor, hydro-extractor, temperature control shaking table, ultrapure water instrument (AD-SR20).
Hydride generation atomic fluorescence method condition determination is: negative high voltage: 340 V; Lamp current: 100 mA; Atomization temperature: 800 ℃; Stove height: 8 mm; Flow rate of carrier gas 500 mL/min; Shield gas flow speed: 1 000mL/min; Time delay: 1 s; Reading duration: 10 s; The liquid feeding time: 8 s; Sampling volume: 2 mL.
Embodiment:
Organic selenium, albumen selenium, polysaccharide selenium or RNA Se content assay method in the selenium-rich rice, described assay method comprises the following steps:
(1) preparation of sample: it is 100 purpose selenium-rich rice dry powder that selenium-rich rice to be detected is pulverized the acquisition granularity, and sealed storage is standby;
1. the extraction of organic selenium: take by weighing above-mentioned selenium-rich rice dry powder 1.00g, add the 10ml ultrapure water, further grinding fully breaks selenium-rich rice dry powder, quantitatively be transferred in the bag filter, the specification of bag filter is 8000Da, with the ultrapure water 24h that dialyses, the centrifugal replacing ultrapure water of every during this time 6h once, dialyzed sample is taken out, and centrifugal 15min obtains precipitation under the 12000rpm condition, and the described vacuum tightness that is deposited in is dry organic selenium m under 60 ℃ the condition for-0.085Mpa, temperature 1G;
2. the extraction of albumen selenium: take by weighing above-mentioned selenium-rich rice dry powder 10.00g, in the 500ml triangular flask, add 0.05mol/LNaOH solution 100ml vibration 2h and get mixed liquor, with mixed liquor centrifugal 15min under the 12000rpm condition, get supernatant, add 0.1mol/LHCl and regulate pH to 5.5, centrifugal 15min must precipitate under the 12000rpm condition once more, and the described vacuum tightness that is deposited in is dry albumen selenium m under 50 ℃ the condition for-0.095Mpa, temperature 2G;
3. the extraction of polysaccharide selenium: take by weighing above-mentioned selenium-rich rice dry powder 2.00g, add 100ml 0.5mol/LNaOH solution, extract polysaccharide in 80 ℃ of water-bath heating 2h, centrifugal 15min under the 12000rpm condition then, getting supernatant washs 3 times with chloroform-butanol solution, remove the floating preteins of polysaccharide, the volume ratio of described chloroform and normal butyl alcohol is 24:1, adding absolute ethyl alcohol to the final concentration of alcohol of solution then is 80%, leave standstill 24h, collecting precipitation, the described vacuum tightness that is deposited in is dry polysaccharide selenium m under 60 ℃ the condition for-0.085Mpa, temperature 3G;
4. the extraction of RNA selenium: take by weighing above-mentioned selenium-rich rice dry powder 10.00g, add 200ml 0.025mol/LNaOH solution shake and swing 45min, transfer pH to 7.0 with 3mol/L hydrochloric acid then, be heated to 90 ℃ after stirring 10min, be cooled to 10 ℃ behind the insulation 10min, in the centrifugal 15min of 12000rpm, get supernatant and transfer pH to 2.5 with 6mol/L hydrochloric acid, 5 ℃ of refrigeration standing over night, once more in the centrifugal 15min of 12000rpm, 1 ~ 2 mass concentration of collecting precipitation adding is 25 ~ 28% ammoniacal liquor, this embodiment adopts 25%, uses the 30ml dissolved in distilled water, washs 3 times with chloroform-butanol solution, the volume ratio of described chloroform and normal butyl alcohol is 24:1, with the water that obtains in vacuum tightness is-0.085Mpa, temperature is that oven dry obtains RNA selenium m under 60 ℃ the condition 4G;
(2) Determination of Selenium Contents
1. typical curve:, as shown in table 1 with reference to the concentration gradient drawing standard curve of GB5009.93-2010 by 0,4,8,12,16,20 μ g/L:
The fluorescent value of table 1 variable concentrations selenium standard solution correspondence
Concentration (μ g/L) 0? 4 8 12 16 20
Fluorescent value 0 220.36 476.54 744.73 1003.76 1245.68
With concentration is horizontal ordinate, and fluorescent value is an ordinate, makes typical curve, as shown in Figure 1, obtains selenium concentration computing formula: Y=63.191X-16.735, R 2=0.9993;
2. digestive juice preparation: take by weighing above-mentioned organic selenium, albumen selenium, polysaccharide selenium and RNA selenium 0.3g respectively in the 50ml triangular flask, add 10ml by HNO 3And HClO 4By volume 4:1 mixed acid mixture, cold digestion is spent the night, next day, hot digestion when solution becomes limpid colourlessly and when occurring with white cigarette, continued to be heated to about residual volume 2ml again, cooling, add 5ml 6mol/L hydrochloric acid again, continue to be heated to solution and become limpid colourless and cooling occurs with white cigarette, transfer is settled to 50ml, obtains digestive juice;
3. measure: get each 2ml of above-mentioned digestive juice respectively in the 10ml color comparison tube, add concentrated hydrochloric acid 2ml, add water and be settled to 10ml, adopt the hydride generation atomic fluorescence method to measure behind the mixing, obtain peak area fluorescent value X successively 1, X 2, X 3,X 4, with peak area fluorescent value X 1, X 2, X 3,X 4Bringing typical curve acquisition organic selenium, albumen selenium, polysaccharide selenium and RNA selenium digestive juice selenium concentration respectively into is Y 1, Y 2, Y 3, Y 4
(3) data processing
1. organic selenium content=Y in the selenium-rich rice 1* 0.25 ÷ 0.3* m 1÷ selenium-rich rice quality, wherein the selenium-rich rice quality is 1.00g;
2. albumen Se content=Y in the selenium-rich rice 2* 0.25 ÷ 0.3* m 2÷ selenium-rich rice quality, wherein the selenium-rich rice quality is 10.00g;
3. polysaccharide Se content=Y in the selenium-rich rice 3* 0.25 ÷ 0.3* m 3÷ selenium-rich rice quality, wherein the selenium-rich rice quality is 2.00g;
4. RNA Se content=Y in the selenium-rich rice 4* 0.25 ÷ 0.3* m 4÷ selenium-rich rice quality, wherein the selenium-rich rice quality is 10.00g.
Total Determination of Selenium Contents is with reference to above-mentioned Se content assay method in the selenium-rich rice, and total selenium, organic selenium, albumen selenium, polysaccharide selenium and RNA Se content see Table 2 in the present embodiment selenium-rich rice.
The total selenium of table 2, organic selenium, albumen selenium, polysaccharide selenium and RNA Se content
Figure 12824DEST_PATH_IMAGE001
The precision test
Take by weighing selenium-rich rice dry powder 0.3g in the 50ml triangular flask, add 10ml by HNO 3And HClO 4By volume 4:1 mixed acid mixture, cold digestion is spent the night, next day, hot digestion when solution becomes limpid colourlessly and when occurring with white cigarette, continued to be heated to about residual volume 2ml again, cooling, add 5ml 6mol/L hydrochloric acid again, continue to be heated to solution and become limpid colourless and cooling occurs with white cigarette, transfer is settled to 50ml, obtains digestive juice;
Get above-mentioned digestive juice 2ml in the 10ml color comparison tube, add concentrated hydrochloric acid 2ml, add water and be settled to 10ml, adopt the hydride generation atomic fluorescence method to measure behind the mixing, obtain peak area fluorescent value X 0, with peak area fluorescent value X 0Bringing typical curve acquisition digestive juice selenium concentration into is Y 0
Total Se content=Y in the selenium-rich rice dry powder 0* 0.25 ÷ 0.3, above-mentioned precision experiment is parallel does 6 groups, the results are shown in Table 3;
The test of table 3 precision
Figure 428762DEST_PATH_IMAGE002
Table 3 shows that 6 the total selenium testing result of parallel sample reappearances are good, and the relative standard deviation is 0.966%, shows that this method has good precision.
The mark-on recovery test
Take by weighing two parts of selenium-rich rice dry powder respectively, every part of 0.30g, the selenium standard solution 6mL of adding 10 μ g/L in every duplicate samples, making the Se content that adds sample is 200 μ g/Kg, adds 10ml by HNO 3And HClO 4By volume 4:1 mixed acid mixture, cold digestion is spent the night, next day, hot digestion when solution becomes limpid colourlessly and when occurring with white cigarette, continued to be heated to about residual volume 2ml again, cooling, add 5ml 6mol/L hydrochloric acid again, continue to be heated to solution and become limpid colourless and cooling occurs with white cigarette, transfer is settled to 50ml, obtains digestive juice;
Get above-mentioned digestive juice 2ml in the 10ml color comparison tube, add concentrated hydrochloric acid 2ml, add water and be settled to 10ml, adopt the hydride generation atomic fluorescence method to measure behind the mixing, obtain peak area fluorescent value X 5And X 6, with peak area fluorescent value X 5And X 6Bringing typical curve acquisition digestive juice selenium concentration into is Y 5And Y 6, concrete data see Table 4.
Table 4 mark-on recovery test
The sample sequence number Total selenium background values (μ g/Kg) Add scalar (μ g/Kg) Measure total value (μ g/Kg) Recovery %
1 206.708 200 419.951 106.62
1 206.708 200 405.952 99.62
Show that by table 4 recovery is 103.12%, illustrate that this method accuracy is good.
Above-described embodiment is a kind of preferable scheme of the present invention, is not that the present invention is done any pro forma restriction, also has other variant and change under the prerequisite that does not exceed the technical scheme that claim puts down in writing.

Claims (5)

1. organic selenium, albumen selenium, polysaccharide selenium or RNA Se content assay method in the selenium-rich rice is characterized in that described assay method comprises the following steps:
(1) preparation of sample: it is 100 purpose selenium-rich rice dry powder that selenium-rich rice to be detected is pulverized the acquisition granularity, and sealed storage is standby;
1. the extraction of organic selenium: take by weighing above-mentioned selenium-rich rice dry powder 1.00g, add 5 ~ 10ml ultrapure water, further grinding fully breaks selenium-rich rice dry powder, quantitatively be transferred in the bag filter, with the ultrapure water 24h that dialyses, dialyzed sample is taken out, and centrifugal 15min obtains precipitation under the 12000rpm condition, and described precipitation vacuum drying gets organic selenium m 1G;
2. the extraction of albumen selenium: take by weighing above-mentioned selenium-rich rice dry powder 10.00g, in the 500ml triangular flask, add 0.05mol/LNaOH solution 100ml vibration 2h and get mixed liquor, with mixed liquor centrifugal 15min under the 12000rpm condition, get supernatant, add 0.1mol/LHCl and regulate pH to 5.5, centrifugal 15min must precipitate under the 12000rpm condition once more, and described precipitation vacuum drying is got albumen selenium m 2G;
3. the extraction of polysaccharide selenium: take by weighing above-mentioned selenium-rich rice dry powder 2.00g, add 100ml 0.5mol/LNaOH solution, extract polysaccharide in 80 ℃ of water-bath heating 2h, centrifugal 15min under the 12000rpm condition gets supernatant and washs 3 times with chloroform-butanol solution then, and the volume ratio of described chloroform and normal butyl alcohol is 24:1, adding absolute ethyl alcohol to the final concentration of alcohol of solution then is 80%, leave standstill 24h, collecting precipitation gets polysaccharide selenium m with described precipitation vacuum drying 3G;
4. the extraction of RNA selenium: take by weighing above-mentioned selenium-rich rice dry powder 10.00g, add 200ml 0.025mol/LNaOH solution shake and swing 45min, transfer pH to 7.0 with 3mol/L hydrochloric acid then, be heated to 90 ℃ after stirring 10min, be cooled to 10 ℃ behind the insulation 10min, in the centrifugal 15min of 12000rpm, get supernatant and transfer pH to 2.5 with 6mol/L hydrochloric acid, 5 ℃ of refrigeration standing over night, once more in the centrifugal 15min of 12000rpm, collecting precipitation adds 1 ~ 2 ammoniacal liquor, use the 30ml dissolved in distilled water, wash 3 times with chloroform-butanol solution, the volume ratio of described chloroform and normal butyl alcohol is 24:1, and the water oven dry that obtains is obtained RNA selenium m 4G;
(2) Determination of Selenium Contents
1. typical curve: by the concentration gradient drawing standard curve of 0,4,8,12,16,20 μ g/L;
2. digestive juice preparation: the organic selenium, albumen selenium, polysaccharide selenium and the RNA selenium 0.3g that take by weighing the said extracted acquisition respectively are in the 50ml triangular flask, add 10ml by HNO3 and HClO4 by volume 4:1 mixed acid mixture, cold digestion is spent the night, next day hot digestion, when solution becomes limpid colourless and when occurring with white cigarette, continue to be heated to about residual volume 2ml again, cooling, add 5ml 6mol/L hydrochloric acid again, continuing to be heated to solution becomes limpid colourless and occur with white cigarette, cooling shifts being settled to 50ml, obtains digestive juice;
3. measure: get each 2ml of above-mentioned digestive juice respectively in the 10ml color comparison tube, add concentrated hydrochloric acid 2ml, add water and be settled to 10ml, adopt the hydride generation atomic fluorescence method to measure behind the mixing, obtain peak area fluorescent value X successively 1, X 2, X 3,X 4, with peak area fluorescent value X 1, X 2, X 3,X 4Bringing typical curve acquisition organic selenium, albumen selenium, polysaccharide selenium and RNA selenium digestive juice selenium concentration respectively into is Y 1, Y 2, Y 3, Y 4
(3) data processing
1. organic selenium content=Y in the selenium-rich rice 1* 0.25 ÷ 0.3* m 1÷ selenium-rich rice quality, wherein the selenium-rich rice quality is 1.00g;
2. albumen Se content=Y in the selenium-rich rice 2* 0.25 ÷ 0.3* m 2÷ selenium-rich rice quality, wherein the selenium-rich rice quality is 10.00g;
3. polysaccharide Se content=Y in the selenium-rich rice 3* 0.25 ÷ 0.3* m 3÷ selenium-rich rice quality, wherein the selenium-rich rice quality is 2.00g;
4. RNA Se content=Y in the selenium-rich rice 4* 0.25 ÷ 0.3* m 4÷ selenium-rich rice quality, wherein the selenium-rich rice quality is 10.00g.
2. organic selenium, albumen selenium, polysaccharide selenium or RNA Se content assay method in the selenium-rich rice according to claim 1 is characterized in that: it is 8000Da that organic selenium extracts the bag filter specification that adopts, ultrapure water of the centrifugal replacing of every 6h in the dialysis procedure.
3. organic selenium, albumen selenium, polysaccharide selenium or RNA Se content assay method in the selenium-rich rice according to claim 1 and 2 is characterized in that: described vacuum drying vacuum tightness is-0.085 ~-0.095Mpa, vacuum drying temperature is 50 ~ 60 ℃.
4. organic selenium, albumen selenium, polysaccharide selenium or RNA Se content assay method is characterized in that in the selenium-rich rice according to claim 1 and 2, and used ammoniacal liquor mass concentration was 25~28% during RNA selenium extracted.
5. organic selenium, albumen selenium, polysaccharide selenium or RNA Se content assay method is characterized in that in the selenium-rich rice according to claim 1 and 2, and hydride generation atomic fluorescence method condition determination is: negative high voltage: 340 V; Lamp current: 100 mA; Atomization temperature: 800 ℃; Stove height: 8 mm; Flow rate of carrier gas 500 mL/min; Shield gas flow speed: 1 000mL/min; Time delay: 1 s; Reading duration: 10 s; The liquid feeding time: 8 s; Sampling volume: 2 mL.
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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104422672A (en) * 2013-08-21 2015-03-18 上海宝钢工业技术服务有限公司 Method for determining content of selenium in soil by adopting microwave digestion-atomic fluorescence technology
CN104655603A (en) * 2015-02-10 2015-05-27 中国农业科学院农产品加工研究所 Identification method for selenium-enriched rice
CN106841138A (en) * 2017-01-17 2017-06-13 广州天科生物科技有限公司 A kind of method of inorganic selenium and organic selenium content in measure Se-enriched yeast
CN107084953A (en) * 2017-04-21 2017-08-22 恩施硒德生物工程有限公司 Method for detecting content of plant-derived organic selenium
CN110057987A (en) * 2019-04-23 2019-07-26 林克鹏 Se-rich grain, grain dust, selenium is qualitative in albumen powder and quantitative identification method
CN111024665A (en) * 2019-12-24 2020-04-17 武汉轻工大学 Method for measuring content of organic selenium in selenium-enriched rice or product prepared from selenium-enriched rice
CN111982874A (en) * 2020-08-14 2020-11-24 奥迈检测有限公司 Method for detecting selenium element in grains
CN114705767A (en) * 2022-03-01 2022-07-05 海南省食品检验检测中心(海南省实验动物中心) Analysis and detection method for selenium form in rice

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102520104A (en) * 2011-12-20 2012-06-27 苏州硒谷科技有限公司 Method for determination of form of selenium in selenium-rich plant material
CN102519933A (en) * 2011-12-20 2012-06-27 苏州硒谷科技有限公司 Method for determining form of selenium in selenium-enriched edible fungi
CN102519930A (en) * 2011-12-20 2012-06-27 苏州硒谷科技有限公司 Method for rapidly determining selenium content in plant sample
CN102830100A (en) * 2012-08-15 2012-12-19 苏州硒谷科技有限公司 Determination method for inorganic selenium and organic selenium in food
CN102928500A (en) * 2012-11-15 2013-02-13 中华人民共和国浙江出入境检验检疫局 Method for detecting organic selenium, protein selenium or polysaccharide selenium in marine products through microwave digestion-ICP-MS (Inductively Coupled Plasma Mass Spectrometry) way

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102520104A (en) * 2011-12-20 2012-06-27 苏州硒谷科技有限公司 Method for determination of form of selenium in selenium-rich plant material
CN102519933A (en) * 2011-12-20 2012-06-27 苏州硒谷科技有限公司 Method for determining form of selenium in selenium-enriched edible fungi
CN102519930A (en) * 2011-12-20 2012-06-27 苏州硒谷科技有限公司 Method for rapidly determining selenium content in plant sample
CN102830100A (en) * 2012-08-15 2012-12-19 苏州硒谷科技有限公司 Determination method for inorganic selenium and organic selenium in food
CN102928500A (en) * 2012-11-15 2013-02-13 中华人民共和国浙江出入境检验检疫局 Method for detecting organic selenium, protein selenium or polysaccharide selenium in marine products through microwave digestion-ICP-MS (Inductively Coupled Plasma Mass Spectrometry) way

Non-Patent Citations (7)

* Cited by examiner, † Cited by third party
Title
刘有芹 等: "大米中硒含量的测定", 《广东微量元素科学》 *
夏新媛 等: "原子荧光法测定富硒米中的硒含量", 《粮油食品科技》 *
张涛 等: "高效液相色谱-等离子体质谱联用方法研究富硒大米中硒的形态", 《分析化学》 *
方建军 等: "富硒大米中硒形态分析", 《食品研究与开发》 *
杨容甫 等: "富硒米中某些化学形态硒含量的测定", 《中山医科大学学报》 *
陈家厚 等: "用微波消解和原子荧光法测定富硒产品中的硒", 《环境科学与管理》 *
韩雪飞 等: "微波消解-原子荧光光谱法测定富硒米中硒的含量", 《河南预防医学杂质》 *

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104422672A (en) * 2013-08-21 2015-03-18 上海宝钢工业技术服务有限公司 Method for determining content of selenium in soil by adopting microwave digestion-atomic fluorescence technology
CN104422672B (en) * 2013-08-21 2018-08-17 上海宝钢工业技术服务有限公司 Using the method for Se content in micro-wave digestion-In Soil With Atomic Fluorescence
CN104655603A (en) * 2015-02-10 2015-05-27 中国农业科学院农产品加工研究所 Identification method for selenium-enriched rice
CN106841138A (en) * 2017-01-17 2017-06-13 广州天科生物科技有限公司 A kind of method of inorganic selenium and organic selenium content in measure Se-enriched yeast
CN106841138B (en) * 2017-01-17 2019-11-26 广州天科生物科技有限公司 A kind of method of inorganic selenium and organic selenium content in measurement Se-enriched yeast
CN107084953A (en) * 2017-04-21 2017-08-22 恩施硒德生物工程有限公司 Method for detecting content of plant-derived organic selenium
CN110057987A (en) * 2019-04-23 2019-07-26 林克鹏 Se-rich grain, grain dust, selenium is qualitative in albumen powder and quantitative identification method
CN111024665A (en) * 2019-12-24 2020-04-17 武汉轻工大学 Method for measuring content of organic selenium in selenium-enriched rice or product prepared from selenium-enriched rice
CN111982874A (en) * 2020-08-14 2020-11-24 奥迈检测有限公司 Method for detecting selenium element in grains
CN114705767A (en) * 2022-03-01 2022-07-05 海南省食品检验检测中心(海南省实验动物中心) Analysis and detection method for selenium form in rice

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