CN101493442A - Method for rapidly measuring selenium content in polysaccharide containing selenium - Google Patents
Method for rapidly measuring selenium content in polysaccharide containing selenium Download PDFInfo
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Abstract
The invention discloses a method for rapidly determining the content of selenium in selenium polysaccharide. The method comprises the following steps: firstly, same volumes of prepared gradient selenium standard solutions are respectively treated to carry out the high-performance liquid chromatography detection, so as to draw standard curves and establish regression equations; secondly, the to-be-tested dry selenium polysaccharide is digested by mixed acid and then diluted into constant volume, so that the to-be-tested sample solution is prepared; thirdly, the sample solution is taken to have the same volume as the treated gradient selenium standard solution and treated with the same conditions, and then the high-performance liquid chromatography test is carried out; and fourthly, based on the established regression equations, the concentration of selenium in the to-be-tested sample solution is calculated and the content of selenium in the dry selenium polysaccharide is further determined. The method overcomes the shortcomings of the previous high-performance liquid chromatography that the sample and the mobile phase are insoluble in the process of determining the selenium content, the linear range is narrow, and the like; and the method has the advantages of accurate and reliable determination result, good repeatability, simplified determination steps, shortened determination time and low determination cost.
Description
Technical field
The present invention relates to the Determination of Selenium Contents method, refer in particular to a kind of method of measuring content of selenium in selenium polysaccharide.
Background technology
Selenium (Se) is the micronutrient element of needed by human, is the natural toxinicide of part heavy metal element, can effectively improve the life immunity function, to anti-cancer, anticancer can playing a significant role.The oxidation resistance of selenium is higher 500 times than vitamin E, so selenium is again antidotal important substance in the human body.Scarce selenium will cause many vitals functions to descend, as cause Keshan disease, brings out hepatonecrosis and angiocardiopathy.Selenium is divided into two kinds of inorganic selenium and organic selenium in the existence form of occurring in nature.The source of organic selenium mainly is the organic selenium such as the selenium polysaccharide of natural selenium-rich plant and synthetic.Selenium polysaccharide has kept the basic configuration and the physiological function of polysaccharide as a kind of organic selenium compounds, but has improved the biology availability of selenium simultaneously and as the physiological function of biological essential trace element, its toxicity and spinoff reduce greatly than inorganic selenium.Studies have shown that that selenium polysaccharide has is anti-oxidant significantly, enhance immunity power, biologically active such as hypoglycemic, anti-ageing, antitumor and antiviral, its activity generally is higher than polysaccharide and inorganic selenium, and to be easier to be that body absorbs and utilizes.
Existing have Determination of Selenium Contents method in the sample: neutron activation analysis method (INAA), atomic emission spectrometry (AES), atomic absorption spectrography (AAS) (AAS), inductively coupled plasma mass spectrometry method (ICP-MS), ultraviolet spectrophotometry and fluorescence spectrophotometry, electrochemical methods etc.Chinese patent CN 101173950A discloses " method for measurement of concentration of selenium diagnosis/determination kit and selenium " on May 7th, 2008, utilizes the content of enzymic colorimetric and enzyme-linked method technical measurement selenium; Chinese patent CN101149357A discloses " a kind of Determination of Selenium Contents method " on March 26th, 2008, can carry out electrochemical analysis mensuration to trace in the water quality or Determination of Trace Selenium; Chinese patent CN 1773254A discloses " selenium assaying liquid and colorimetric cylinder thereof " on May 17th, 2006, can measure the content of selenium in the water quality.In above-mentioned method of testing and the technology, testing procedure is often comparatively loaded down with trivial details, and analytical cycle is long, has limited its range of application; The assay method that has exists that measurement result is inaccurate, the shortcoming of poor repeatability.Document " chelate extraction before the post-high effective liquid chromatography for measuring Determination of Trace Selenium " (analytical chemistry, 1988,16 (4) 328～330) reported HPLC to Se content in the natural drug (following be called for short " high performance liquid chromatography ") assay method with HPLC, but exist the range of linearity narrower (2～8ng), shortcoming such as cyclohexane and moving phase acetonitrile be immiscible.At present the mensuration to content of selenium in selenium polysaccharide also only limits to said method, the method for more quick, accurate, universal mensuration content of selenium in selenium polysaccharide that people expect to have.
Summary of the invention
Technical matters to be solved by this invention provides a kind of method of fast, accurately measuring content of selenium in selenium polysaccharide.
For solving the problems of the technologies described above, the present invention is a kind of fast, accurately measure the method for content of selenium in selenium polysaccharide, comprises the steps:
(1) drawing standard curve and set up regression equation: the selenium standard solution mother liquor of getting respective volume respectively constant volume in the volumetric flask of same capacity, the concentration of described selenium standard solution mother liquor is 50～500ug/ml, the volumetric flask of described same capacity is capacity 10ml or above volumetric flask, the gradient selenium standard solution of concentration range 0.005～1ug/ml is made in dilution successively, get each gradient selenium standard solution of 10ml respectively and add the EDTA-2Na solution of 0.2mol/L and each 2～4ml of oxammonium hydrochloride of 0.5mol/L, leave standstill 5～10min after the vibration evenly, the dark place add respectively 0.1% 2,3-diaminonaphthalene (2, the 3-diaminonaphthalene hereinafter is called for short DAN with it in the present invention and substitutes) solution 2～4ml, boiling water bath 4～6min, after taking-up is cooled to room temperature, add cyclohexane 5ml, fully oscillation extraction is got the cyclohexane layer and is injected the high performance liquid chromatography detection, and each sample size is 20ul, each sample repeats three pins, with peak area mean value to gradient selenium concentration of standard solution drawing standard curve and set up regression equation;
(2) clearing up of testing sample: take by weighing dry selenium polysaccharide to be measured, add the nitration mixture of respective amount, the ratio of described dry selenium polysaccharide and described nitration mixture is a weight: volume=0.01～0.03g: 2ml, the volume ratio of each composition is HNO in the described nitration mixture
3: H
2SO
4: HClO
4=1: 1: 4, cleared up in 135 ℃ 1～2 hour the static back of spending the night, and gets digestion solution A;
(3) processing of digestion solution and HPLC method detect: is in 10ml or above volumetric flask, the concentration range 0.005～1ug/ml of the selenium concentration of the sample solution of institute constant volume in step (1) prepared gradient selenium standard solution in the distilled water diluting constant volume in capacity with digestion solution A; Specifically, if this digestion solution A dilution is settled in the concentration range 0.005～1ug/ml of its selenium concentration prepared gradient selenium standard solution in step (1) behind the 10ml, then with the sample solution of this 10ml sample solution as next step processing; If dry sample to be measured is the higher sample of selenium content, then can expand as suitable volume to volume after the dilution of digestion solution A as being settled to 100ml or 1000ml etc., make in the concentration range 0.005～1ug/ml of its selenium concentration prepared gradient selenium standard solution in step (1), get the sample solution of this sample solution of 10ml again as next step processing; According to handling this 10ml sample solution with the middle identical experiment condition of 10ml gradient selenium standard solution of handling of step (1), promptly add the EDTA-2Na solution of 0.2mol/L and each 2～4ml of oxammonium hydrochloride of 0.5mol/L, leave standstill 5～10min after the vibration evenly, the dark place adds DAN solution 2～4ml of 0.1%, boiling water bath 4～6min, after taking-up is cooled to room temperature, add cyclohexane 5ml, abundant oscillation extraction, get the cyclohexane layer and inject the high performance liquid chromatography detection, each sample size is 20ul, each sample repeats into three pins, the regression equation of being set up in the peak area mean value substitution step (1) is calculated the selenium concentration (ug/ml) of sample solution behind the constant volume, and the weight that contains the total amount of selenium and used dry selenium polysaccharide according to the sample solution of institute's constant volume is calculated the Se content (ug/g) of the dry selenium polysaccharide of surveying again.
Aforesaid realization step of the present invention: in step (1), described selenium standard solution mother liquor is the selenium standard solution of 100ug/ml, the volumetric flask of described same capacity is the volumetric flask of 10ml, and the gradient selenium standard solution of described concentration range 0.005～1ug/ml is respectively the gradient selenium standard solution of 0.005ug/ml, 0.025ug/ml, 0.05ug/ml, 0.25ug/ml, 0.5ug/ml and 1ug/ml; In step (2), the dry selenium polysaccharide weight to be measured that is taken by weighing is 0.02g, and the nitration mixture volume that is added is 2ml.
The high performance liquid chromatography parameter:
Chromatographic column: C18 ODS post;
Eluant, eluent: methyl alcohol: the volume ratio of ethanol=60%: 40%;
Elution rate: 0.8ml/min;
Column temperature: 30 ℃;
Fluorescence detector detects: excitation wavelength 374nm, emission wavelength 555nm;
Sample size: 20ul;
Retention time: 2.5～3.5min;
The range of linearity of typical curve: 0.005～1ug/ml;
Detection limit: 5ng/g.
Table 1 is the typical curve data of embodiment 1～3, and Fig. 1～3 are respectively the typical curve of with peak area (X) gradient selenium concentration of standard solution (Y) being drawn among the embodiment 1～3, the regression equation of the correspondence of being set up, the R of its coefficient R in embodiment 1～3
2Value all approaches 1, illustrates that its corresponding regression equation all has extremely significant linear dependence relation.
The pairing HPLC detected peaks of each gradient selenium standard solution area among table 1 embodiment 1～3
Reach the R of the regression equation of setting up among each embodiment
2Value
| Se content (ug/ml) | Embodiment 1 peak area | Embodiment 2 peak areas | Embodiment 3 peak areas |
| 0.005 | 0.962 | 0.528 | 0.357 |
| 0.025 | 1.854 | 1.554 | 1.393 |
| 0.05 | 2.852 | 2.813 | 2.669 |
| 0.25 | 13.498 | 13.422 | 12.843 |
| 0.5 | 27.005 | 25.369 | 23.936 |
| 1 | 55.363 | 53.910 | 51.543 |
| R 2 | 0.99979 | 0.99955 | 0.99937 |
Table 2 has provided at the Se content of same sample copy inventive embodiments mensuration and the comparison of the Se content data that ICP (inductively coupled plasma emission spectrography) measures; ICP mensuration herein is in other mechanism for testing mensuration, and it is relatively more accurate, reliable at present assay method that ICP measures, but is difficult to popularize because of testing expense is higher; The measurement result of the embodiment of the invention and ICP measurement result basically identical illustrate that measurement result of the present invention is accurately, reliably.
The HPLC of table 2 embodiment of the invention measures the corresponding dry sample Se content of measuring with ICP (ug/g) and compares
| The embodiment sample | The peak area mean value of HPLC working sample | The Se content of HPLC working sample (ug/g) | The Se content of ICP working sample (ug/g) |
| Embodiment 1 sample a | 40.765 | 371.0 | 361.7 |
| Embodiment 2 sample b | 17.586 | 167.5 | 159.3 |
| Embodiment 3 sample c | 14.955 | 1475.0 | 1467.4 |
The invention has the beneficial effects as follows: in the method for a kind of fast measuring content of selenium in selenium polysaccharide of the present invention, the intermiscibility of the mixed liquor of cyclohexane and mobile phase methanol and ethanol is fine, typical curve range of linearity broad, has overcome in the past shortcomings such as HPLC measures in the Se content process sample and moving phase is immiscible, the range of linearity is narrower; The inventive method testing result accurately and reliably, good reproducibility has been simplified the detection step greatly, does not comprise the pretreated time of Specimen eliminating, the time that sample is once measured only is about 20 minutes, to have saved minute, the mensuration expense is low, is easy to promotion and implementation.
Description of drawings
Below in conjunction with the drawings and specific embodiments the present invention is described in further detail:
Fig. 1 is the typical curve according to data creating among the embodiment 1;
Fig. 2 is the typical curve according to data creating among the embodiment 2;
Fig. 3 is the typical curve according to data creating among the embodiment 3;
Fig. 4 is the liquid chromatogram of the specimen solution of embodiment 1, wherein horizontal ordinate be retention time (minute), ordinate is that fluorescence signal intensity is response (MV).
Embodiment
The following examples can illustrate in greater detail the present invention, but do not limit the present invention in any form.
The purpose of this invention is to provide a kind of method of fast, accurately measuring Se content in the selenium polysaccharide sample.In practical measurement, the same batch sample of every survey requires typical curve to make again.
Embodiment 1
The purpose of this invention is to provide a kind of method of fast, accurately measuring Se content in the selenium polysaccharide sample:
(1) drawing standard curve and set up regression equation: the selenium standard solution that with concentration is 100ug/ml is a mother liquor, this mother liquor constant volume that therefrom takes out respective volume respectively is in the volumetric flask of 10ml, successively according to 0.005ug/ml, 0.025ug/ml, 0.05ug/ml, 0.25ug/ml, 0.5ug/ml and the concentration dilution of 1ug/ml is made new serial gradient selenium standard solution, respectively each selenium standard solution of 10ml is added the EDTA-2Na solution of 0.2mol/L and each 2ml of oxammonium hydrochloride of 0.5mol/L, leave standstill 5min after the vibration evenly, the dark place adds 0.1% DAN solution 4ml respectively, boiling water bath 5min, after taking-up is cooled to room temperature, add cyclohexane 5ml, abundant oscillation extraction, get the cyclohexane layer and inject the high performance liquid chromatography detection, each sample size is 20ul, each sample repeats three pins, with peak area mean value to gradient selenium concentration of standard solution drawing standard curve (Fig. 1) and set up regression equation: Y=0.0183X-0.00401, R
2=0.99979;
(2) clearing up of testing sample: take by weighing dry selenium polysaccharide sample a 0.02g to be measured, add nitration mixture 2ml, the volume ratio of each composition is HNO in the described nitration mixture
3: H
2SO
4: HClO
4=1: 1: 4, cleared up in 135 ℃ 1 hour the static back of spending the night, and gets digestion solution A;
(3) processing of digestion solution and HPLC method detect: with digestion solution A distilled water diluting constant volume, this digestion solution A dilution is settled to 10ml (its selenium concentration is in the concentration range 0.005～1ug/ml of above-mentioned gradient selenium standard solution), this 10ml sample solution is added the EDTA-2Na solution of 0.2mol/L and each 2ml of oxammonium hydrochloride of 0.5mol/L, leave standstill 5min after the vibration evenly, the dark place adds 0.1% DAN solution 4ml, boiling water bath 5min, after taking-up is cooled to room temperature, add cyclohexane 5ml, abundant oscillation extraction, get the cyclohexane layer and inject high performance liquid chromatography detection (liquid chromatogram such as Fig. 4), each sample size is 20ul, each sample repeats into three pins, the regression equation of being set up in the test sample product a of the institute peak area mean value 40.765 substitution steps (1) (Y=0.0183X-0.00401) calculated the sample solution selenium concentration is 0.742ug/ml behind the constant volume, the Se content that calculates the dry selenium polysaccharide of surveying according to the weight 0.02g of total amount 7.42ug that contains selenium in the 10ml institute constant volume sample solution and used dry selenium polysaccharide is 371.0ug/g again.
Embodiment 2
The purpose of this invention is to provide a kind of method of fast, accurately measuring Se content in the selenium polysaccharide sample:
(1) drawing standard curve and set up regression equation: the selenium standard solution that with concentration is 100ug/ml is a mother liquor, this mother liquor constant volume that therefrom takes out respective volume respectively is in the volumetric flask of 10ml, successively according to 0.005ug/ml, 0.025ug/ml, 0.05ug/ml, 0.25ug/ml, 0.5ug/ml and the concentration dilution of 1ug/ml is made new serial gradient selenium standard solution, respectively each selenium standard solution of 10ml is added the EDTA-2Na solution of 0.2mol/L and each 4ml of oxammonium hydrochloride of 0.5mol/L, leave standstill 10min after the vibration evenly, the dark place adds 0.1%DAN solution 2ml respectively, boiling water bath 4min, after taking-up is cooled to room temperature, add cyclohexane 5ml, abundant oscillation extraction, get the cyclohexane layer and inject the high performance liquid chromatography detection, each sample size is 20ul, each sample repeats three pins, with peak area mean value to gradient selenium concentration of standard solution drawing standard curve (Fig. 2) and set up regression equation: Y=0.0188X+0.00487, R
2=0.99955;
(2) clearing up of testing sample: take by weighing dry selenium polysaccharide sample b 0.02g to be measured, add nitration mixture 2ml, the volume ratio of each composition is HNO in the described nitration mixture
3: H
2SO
4: HClO
4=1: 1: 4, cleared up in 135 ℃ 1.5 hours the static back of spending the night, and gets digestion solution A;
(3) processing of digestion solution and HPLC method detect: with digestion solution A distilled water diluting constant volume, this digestion solution A dilution is settled to 10ml (its selenium concentration is in the concentration range 0.005～1ug/ml of above-mentioned gradient selenium standard solution), this 10ml sample solution is added the EDTA-2Na solution of 0.2mol/L and each 4ml of oxammonium hydrochloride of 0.5mol/L, leave standstill 10min after the vibration evenly, the dark place adds 0.1% DAN solution 2ml, boiling water bath 4min, after taking-up is cooled to room temperature, add cyclohexane 5ml, abundant oscillation extraction, concentration is followed successively by 2ug/ml in the cyclohexane, 1ug/ml, 0.5ug/ml, 0.1ug/ml, 0.05ug/ml and 0.01ug/ml, get the cyclohexane layer and inject the high performance liquid chromatography detection, each sample size is 20ul, each sample repeats into three pins, the regression equation of being set up in the test sample product b of the institute peak area mean value 17.586 substitution steps (1) (Y=0.0188X+0.00487) calculated the selenium concentration of sample solution is 0.335ug/ml behind the constant volume, the Se content that calculates the dry selenium polysaccharide of surveying according to the weight 0.02g of total amount 3.35ug that contains selenium in the 10ml institute constant volume sample solution and used dry selenium polysaccharide is 167.5ug/g again.
Embodiment 3
The purpose of this invention is to provide a kind of method of fast, accurately measuring Se content in the selenium polysaccharide sample:
(1) drawing standard curve and set up regression equation: the selenium standard solution that with concentration is 100ug/ml is a mother liquor, this mother liquor constant volume that therefrom takes out respective volume respectively is in the volumetric flask of 10ml, successively according to 0.005ug/ml, 0.025ug/ml, 0.05ug/ml, 0.25ug/ml, 0.5ug/ml and the concentration dilution of 1ug/ml is made new serial gradient selenium standard solution, respectively each selenium standard solution of 10ml is added the EDTA-2Na solution of 0.2mol/L and each 3ml of oxammonium hydrochloride of 0.5mol/L, leave standstill 8min after the vibration evenly, the dark place adds 0.1%DAN solution 3ml respectively, boiling water bath 6min, after taking-up is cooled to room temperature, add cyclohexane 5ml, abundant oscillation extraction, get the cyclohexane layer and inject the high performance liquid chromatography detection, each sample size is 20ul, each sample repeats three pins, with peak area mean value to gradient selenium concentration of standard solution drawing standard curve (Fig. 3) and set up regression equation: Y=0.0196X+0.00161, R
2=0.99937;
(2) clearing up of testing sample: take by weighing dry selenium polysaccharide sample c 0.02g to be measured, add nitration mixture 2ml, the volume ratio of each composition is HNO in the described nitration mixture
3: H
2SO
4: HClO
4=1: 1: 4, cleared up in 135 ℃ 2 hours the static back of spending the night, and gets digestion solution A;
(3) processing of digestion solution and HPLC method detect: with digestion solution A distilled water diluting constant volume, this digestion solution A dilution is settled to 100ml (its selenium concentration is in the concentration range 0.005～1ug/ml of above-mentioned gradient selenium standard solution), get this sample solution of 10ml and add the EDTA-2Na solution of 0.2mol/L and each 3ml of oxammonium hydrochloride of 0.5mol/L, leave standstill 8min after the vibration evenly, the dark place adds 0.1% DAN solution 3ml, boiling water bath 6min, after taking-up is cooled to room temperature, add cyclohexane 5ml, abundant oscillation extraction, get the cyclohexane layer and inject the high performance liquid chromatography detection, each sample size is 20ul, each sample repeats into three pins, the concentration of the regression equation of being set up in the test sample product c of the institute peak area mean value 14.955 substitution steps (1) (Y=0.0196X+0.00161) being calculated the selenium in the sample solution behind the constant volume is 0.295ug/ml, and to calculate the Se content of dry selenium polysaccharide be 1475.0ug/g to the root 100ml institute constant volume sample solution weight 0.02g that contains the total amount 29.5ug of selenium and used dry selenium polysaccharide again.
Claims (2)
1. the method for a fast measuring content of selenium in selenium polysaccharide is characterized in that may further comprise the steps:
(1) drawing standard curve and set up regression equation: the selenium standard solution mother liquor of getting respective volume respectively constant volume in the volumetric flask of same capacity, the concentration of described selenium standard solution mother liquor is 50～500ug/ml, the volumetric flask of described same capacity is capacity 10ml or above volumetric flask, the gradient selenium standard solution that concentration range is 0.005～1ug/ml is made in dilution successively, get each gradient selenium standard solution of 10ml respectively and add the EDTA-2Na solution of 0.2mol/L and each 2～4ml of oxammonium hydrochloride of 0.5mol/L, leave standstill 5～10min after the vibration evenly, the dark place add respectively 0.1% 2,3-diaminonaphthalene solution 2～4ml, boiling water bath 4～6min, after taking-up is cooled to room temperature, add cyclohexane 5ml, abundant oscillation extraction, get the cyclohexane layer and inject high performance liquid chromatography and detect, with peak area mean value to gradient selenium concentration of standard solution drawing standard curve and set up regression equation;
(2) clearing up of testing sample: take by weighing dry selenium polysaccharide to be measured, add nitration mixture, the ratio of described dry selenium polysaccharide and described nitration mixture is a weight: volume=0.01～0.03g: 2ml, the volume ratio of each composition is HNO in the described nitration mixture
3: H
2SO
4: HClO
4=1: 1: 4, cleared up in 135 ℃ 1～2 hour the static back of spending the night, and gets digestion solution A;
(3) processing of digestion solution and high performance liquid chromatography detect: with digestion solution A with the distilled water diluting constant volume in capacity 10ml or above volumetric flask, in the concentration range 0.005～1ug/ml of the selenium concentration of the sample solution of institute's constant volume prepared gradient selenium standard solution in step (1), get this sample solution of 10ml according to handling with the identical experiment condition of the middle 10ml of processing of step (1) gradient selenium standard solution, promptly add the EDTA-2Na solution of 0.2mol/L and each 2～4ml of oxammonium hydrochloride of 0.5mol/L, leave standstill 5～10min after the vibration evenly, 2 of dark place adding 0.1%, 3-diaminonaphthalene solution 2～4ml, boiling water bath 4～6min, after taking-up is cooled to room temperature, add cyclohexane 5ml, abundant oscillation extraction, get the cyclohexane layer and inject the high performance liquid chromatography detection, the regression equation of being set up in the peak area mean value substitution step (1) is calculated the selenium concentration of sample solution behind the constant volume, and the weight that contains the total amount of selenium and used dry selenium polysaccharide to be measured according to the sample solution of institute's constant volume is calculated the Se content of the dry selenium polysaccharide of surveying again.
2. the method for a kind of fast measuring content of selenium in selenium polysaccharide according to claim 1, the step of implementing this method is identical with the described step of claim 1, it is characterized in that: in step (1), described selenium standard solution mother liquor is the selenium standard solution of 100ug/ml, the volumetric flask of described same capacity is the volumetric flask of 10ml, the gradient selenium standard solution of described concentration range 0.005～1ug/ml is respectively 0.005ug/ml, 0.025ug/ml, 0.05ug/ml, 0.25ug/ml, 0.5ug/ml and the gradient selenium standard solution of 1ug/ml, it is the mixed liquor of methyl alcohol and ethanol that described high performance liquid chromatography detects used eluant, eluent, methyl alcohol: the volume ratio of ethanol=60%: 40%; In step (2), the dry selenium polysaccharide weight to be measured that is taken by weighing is 0.02g, and the nitration mixture volume that is added is 2ml.
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| 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 |
| CN102519932A (en) * | 2011-12-20 | 2012-06-27 | 苏州硒谷科技有限公司 | Rapid detection method of selenium content in animal tissues |
| CN102519931A (en) * | 2011-12-20 | 2012-06-27 | 苏州硒谷科技有限公司 | Method for rapid determination of content of selenium in soil sample |
| CN101620210B (en) * | 2009-08-12 | 2012-11-14 | 西北师范大学 | Method for rapidly detecting sulphur content in polysaccharide sulfate |
| 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 |
| CN106248646A (en) * | 2016-09-09 | 2016-12-21 | 哈尔滨中科龙祥科技有限公司 | A kind of method of Se content in Accurate Determining wine |
| CN106323933A (en) * | 2016-08-12 | 2017-01-11 | 浙江大学 | Method for determining elementary selenium content |
| CN111855847A (en) * | 2020-07-08 | 2020-10-30 | 浙江大学 | Method for determining total selenium content in selenium-enriched proteoglycan by high performance liquid chromatography |
| CN115047110A (en) * | 2022-06-17 | 2022-09-13 | 陕西科技大学 | Rapid detection method of selenium polysaccharide in selenium-rich beans |
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2009
- 2009-02-23 CN CNA2009100091955A patent/CN101493442A/en active Pending
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| CN101620210B (en) * | 2009-08-12 | 2012-11-14 | 西北师范大学 | Method for rapidly detecting sulphur content in polysaccharide sulfate |
| 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 |
| CN102519932A (en) * | 2011-12-20 | 2012-06-27 | 苏州硒谷科技有限公司 | Rapid detection method of selenium content in animal tissues |
| CN102519931A (en) * | 2011-12-20 | 2012-06-27 | 苏州硒谷科技有限公司 | Method for rapid determination of content of selenium in soil sample |
| 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 |
| CN103884785B (en) * | 2013-12-09 | 2016-03-16 | 恩施土家族苗族自治州农业科学院 | A kind of detection method of selenium |
| CN106323933A (en) * | 2016-08-12 | 2017-01-11 | 浙江大学 | Method for determining elementary selenium content |
| CN106248646A (en) * | 2016-09-09 | 2016-12-21 | 哈尔滨中科龙祥科技有限公司 | A kind of method of Se content in Accurate Determining wine |
| CN111855847A (en) * | 2020-07-08 | 2020-10-30 | 浙江大学 | Method for determining total selenium content in selenium-enriched proteoglycan by high performance liquid chromatography |
| CN115047110A (en) * | 2022-06-17 | 2022-09-13 | 陕西科技大学 | Rapid detection method of selenium polysaccharide in selenium-rich beans |
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