CN102928500B - Method for detecting organic selenium, protein selenium or polysaccharide selenium in marine products through microwave digestion-ICP-MS (Inductively Coupled Plasma Mass Spectrometry) way - Google Patents
Method for detecting organic selenium, protein selenium or polysaccharide selenium in marine products through microwave digestion-ICP-MS (Inductively Coupled Plasma Mass Spectrometry) way Download PDFInfo
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- CN102928500B CN102928500B CN201210458379.1A CN201210458379A CN102928500B CN 102928500 B CN102928500 B CN 102928500B CN 201210458379 A CN201210458379 A CN 201210458379A CN 102928500 B CN102928500 B CN 102928500B
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Abstract
The invention relates to a detection method based on selenium form analysis in marine products, in particular to a method for detecting organic selenium, protein selenium or polysaccharide selenium in marine products through microwave digestion-inductively coupled plasma mass spectrometry (ICP-MS) way. The method for detecting organic selenium, protein selenium or polysaccharide selenium in marine products through microwave digestion-ICP-MS way comprises steps as follows: 1, preparing a sample: removing shell of the sample, storing into a sample bag; (1) separating and purifying organic selenium: carrying out a continuous dialysis method to separate and purify the organic selenium; (2) separating and purifying protein selenium; and (3) separating and purifying polysaccharide selenium; and 2, detecting the content of selenium: (1) performing microwave digestion; (2) implementing blank test: processing an agent without being contacted with a sample to be detected according to the method in sub-step (1) of step 2; and (3) detecting by inductively coupled plasma mass spectrometry. The method has the advantages that the organic selenium, the protein selenium or the polysaccharide selenium in the marine products can be efficiently, simply, conveniently and quickly detected.
Description
Technical field
The present invention relates to the detection method that in marine product, Se form is analyzed, particularly relate to a kind of detection method using micro-wave digestion-inductivity coupled plasma mass spectrometry (ICP-MS) method directly to measure Organic Selenium in marine product, albumen selenium or polysaccharide selenium.
Background technology
Trace elements of selenium is the required nutrient of biosome, but but excessive selenium can cause poisoning, and therefore, selenium is the element with useful and poisonous double properties, takes in too much or insufficiency of intake all can cause body injury, gives rise to diseases.Due to selenium helpfulness and causing toxicity between concentration limit very narrow, the day recommended intake of selenium is limited in 50-200 μ g/d.In addition, the dual character of selenium is relevant with the form that it exists and content thereof.
The existing forms of selenium is mainly divided into inorganic selenium and Organic Selenium, the functional chemical form depended on existing for it of selenium.In physical environment, selenium mainly exists with inorganic forms, and common are sodium selenite and sodium selenate, reduced levels just has very high toxicity, and absorptivity is low, and only have few part to be absorbed by body, major part is all discharged with urine, and bioavailability is low.Selenium mainly exists with organic form in vivo, mainly comprises the biomacromolecule such as albumen selenium, polysaccharide selenium.Relative to toxicity and the mutagenesis of inorganic selenium; Organic Selenium toxicity is low, spinoff is little, digestibility and biology utilization factor high; its Biomedical function is greater than inorganic selenium; as albumen selenium has Cell protection from important physiological function such as lipid peroxidation, scavenging free radicals, regulation and control hormones, polysaccharide selenium have improve immune, anti-oxidant, anti-metal is poisoning, the effect of inhibiting tumor cell and virus.The selenium of visible different shape is different to the effect of biosome, the different physiology of selenium compound, biologically active and transportion and transformation thereof, not only depend on the total concentration level of selenium, and directly related with the concentration level of selenide under the chemical form that selenium exists and different chemical form.China is one and existingly enriches selenium resource, there is again the country in large area selenium deficiency area, and an important diet source of marine product to be people obtain selenium.
At present, both at home and abroad about the research of the occurrence patterns analysis of selenium in marine product rarely has report.The detection method both at home and abroad directly measuring Organic Selenium in marine product, albumen selenium and polysaccharide selenium about micro-wave digestion-ICP-MS method there is not yet bibliographical information.Therefore, carry out the detection method research of Organic Selenium in marine product, albumen selenium and polysaccharide selenium, verify the occurrence patterns of selenium in marine product and content distribution further, the understanding to marine product nutritive value to marine product safety and raising, to promoting the exploitation of marine product and development and foreign trade, all significant to instructing people rationally to mend selenium.
Summary of the invention
In order to solve the difficult problem that in marine product, Se form analysis detects, the object of this invention is to provide a kind of detection method utilizing micro-wave digestion-inductively coupled plasma mass spectrometry directly to measure Organic Selenium in marine product, albumen selenium or polysaccharide selenium, the method has sensitive, accurate, quick, easy feature.
To achieve these goals, present invention employs following technical scheme:
Micro-wave digestion-ICP-MS method directly measures the detection method of Organic Selenium in marine product, albumen selenium or polysaccharide selenium, and the method comprises the following steps:
One, the preparation of sample
Shelled by sample, all edible part hollanders fully blend and mix, and load sample sack, for subsequent use-18 DEG C of storages;
(1) separation and purification of Organic Selenium
Adopt and continue dialysis, accurately take 20.0g test portion and load in bag filter, dialyse 96h in ultrapure water, changes a water every 12h; Test portion after having dialysed is through vacuum freeze drying, for subsequent use-18 DEG C of storages;
(2) separation and purification of selenoprotein
1) accurately take 20.0g test portion in beaker, add 120mL acetone, be placed on magnetic stirring apparatus and stir degreasing 4h, the centrifugal 15min of 8500r/min, abandons supernatant;
2) after volatilizing acetone, add 600mL 0.25mol/L NaOH solution, 50 DEG C of stirring in water bath extract 4h, filter, obtain supernatant;
3) filter residue adds 200mL 0.25mol/L NaOH solution and repeatedly extracts 2 times, merging filtrate, and adding ammonium sulfate to saturation degree is 95%, 4 DEG C of standing 12h;
4) the centrifugal 25min of 8000r/min, precipitates with 50mL50mmol/L trishydroxymethylaminomethane-HCl damping fluid, pH8.0, dissolves;
5) at 4 DEG C successively with 50mmol/L trishydroxymethylaminomethane-HCl damping fluid, ultrapure water dialysis to BaCl
2solution detects in dislysate without SO
4 2-separate out;
6) test portion after having dialysed through vacuum freeze drying ,-18 DEG C of storages, for Selenium Contents;
(3) separation and purification of selenium polysaccharide
1) Thick many candies extracts: accurately take 20.0g test portion in beaker, after degreasing, add 500mL deionized water, 70 DEG C of water-bath lixiviate 5h, the centrifugal 15min of 8500r/min, collects supernatant; Add 3 times of volume 95% ethanol, 4 DEG C of hold over night, centrifugal collecting precipitation; Precipitate with deionized water is redissolved, and freeze drying obtains Thick many candies;
2) de-albumen: adopt trypsase+Sevag method to take off albumen, regulate pH to 6.5, add the trypsase of 4% Thick many candies, hatch 6h for 60 DEG C; 100 DEG C of boiling water heating 5min deactivation; Centrifuging and taking supernatant, adds 1/3 chloroform-normal butyl alcohol, and volume ratio is 4:1, fully rocks 30min, stratification, collects upper strata liquid glucose, repeatedly until middle layer is separated out without metaprotein; Liquid glucose 3 times of volume 95% ethanol, 4 DEG C of hold over night, obtain polysaccharide precipitation, and after centrifugal, polysaccharide precipitation 85% ethanol is washed 3 times, vacuum freeze drying obtains polysaccharide, for Selenium Contents;
Two, the mensuration of Se content
(1) micro-wave digestion
Accurately take 0.2g respectively, Organic Selenium, selenoprotein or selenium polysaccharide that test portion or extraction obtain, add 5mL HNO
3with 2mL H
2o
2, put into microwave dissolver and carry out micro-wave digestion.After Specimen eliminating completes, be cooled to room temperature, digestion solution be transferred in 100mL volumetric flask, add 1 μ g/mL respectively
72ge and
89in Y is two, mark uses solution 40 μ L, is settled to scale, shakes up with water, to be measured;
Micro-wave digestion program is as follows: power 1200W, step 1,120 DEG C, intensification 5min, keeps 5min; Step 2,180 DEG C, intensification 15min, keeps 10min;
(2) blank test
According to the reagent that (one) method process in two contacts with testing sample;
(3) inductivity coupled plasma mass spectrometry measures
Inductivity coupled plasma mass spectrometry condition determination is as follows:
1) RF emissive power: 1.30KW;
2) cooling gas flow: 13.0L/min;
3) atomization gas flow: 0.81L/min;
4) assisted gas flow: 0.78L/min;
5) atomizer: concentric atomizer;
6) spray chamber temperature: 3 DEG C;
7) sampling spiroid/intercepting cone: Nickel;
8) quadrupole rod bias voltage :-13.00 V;
9) sextupole bar bias voltage :-11 V;
10) sampling depth: 120 mm;
11) gas (7%H2:93%He) is collided: 6 mL/min;
12) sampling pattern: entirely quantitative;
13) scan mode: jump peak;
14) integral time: 15 ms;
15) measurement is counted: 3;
16) lifting capacity: 1 mL/min;
17) quality monitoring number: 80.
The present invention, owing to have employed above-mentioned technical scheme, by optimizing every location parameter of micro-wave digestion condition and ICP-MS, adopts
72ge and
89y corrects as two interior mark, differential technique, adopt crash response pool mode (CCT), discriminate against technology (KED) with the use of kinetic energy and eliminate the interference of isobar, multi-atomic ion and multiple-charged ion, can efficient, easy, measure Organic Selenium, albumen selenium and polysaccharide selenium in marine product fast.Detecting of selenium is limited to 0.006 μ g/L, mensuration lower bound is 3 μ g/kg.
Embodiment
The following specific embodiments of the present invention is to make a detailed explanation.
Micro-wave digestion-inductively coupled plasma mass spectrometry of the present invention directly measures the detection method of Organic Selenium in marine product, albumen selenium and polysaccharide selenium, and the method comprises the following steps:
one, the preparation of sample
Shelled by sample, all edible part hollanders fully blend and mix, and load sample sack, at-18 DEG C of storage (works for subsequent use
For test portion).
(1) separation and purification of Organic Selenium
Adopting and continue dialysis, accurately take 20.0g(and to be accurate to after radix point four) test portion loads in bag filter, at ultrapure water
Middle dialysis 96h(is to remove Small molecular), change a water every 12h.Test portion after having dialysed is through vacuum freeze drying, for subsequent use-18 DEG C of storages.
(2) separation and purification of selenoprotein
Accurately take 20.0g(be accurate to radix point after four) add 120mL acetone in test portion to beaker, be placed on magnetic agitation
Device stirs degreasing 4h, the centrifugal 15min of 8500r/min, abandons supernatant.After volatilizing acetone, add 600mL 0.25mol/L
NaOH solution, stirred at ambient temperature extracts 4 hours, filters, obtains supernatant.Filter residue adds 200mL 0.25mol/L NaOH solution and repeatedly extracts 2 times, merging filtrate, and adding ammonium sulfate to saturation degree is 95%, 4 DEG C of standing 12h.The centrifugal 25min of 8000r/min, precipitates and dissolves with 50mL50mmol/L trishydroxymethylaminomethane-HCl damping fluid (pH8.0).50mmol/L trishydroxymethylaminomethane-HCl damping fluid (pH8.0), ultrapure water is used to dialyse to BaCl at 4 DEG C successively
2solution detects in dislysate without SO
4 2-separate out (to remove other Small molecular).Test portion after having dialysed through vacuum freeze drying ,-18 DEG C of storages, for Selenium Contents.
(3) separation and purification of selenium polysaccharide
(1) Thick many candies extracts: accurately take 20.0g(and to be accurate to after radix point four) test portion in beaker, after degreasing, add
Enter 500mL deionized water, 75 DEG C of water-bath lixiviate 5h, the centrifugal 15min of 8500r/min, collect supernatant.Add 3 times of volume 95% ethanol, 4 DEG C of hold over night, centrifugal collecting precipitation.Precipitate with deionized water is redissolved, and freeze drying obtains Thick many candies.
(2) de-albumen: adopt trypsase+Sevag method to take off albumen, regulate pH to 6.5, add the pancreas egg of 4% Thick many candies
White enzyme, hatches 6h for 60 DEG C.100 DEG C of boiling water heating 5min deactivation.Centrifuging and taking supernatant, adds 1/3 chloroform-normal butyl alcohol (4:1, V/V), fully rocks 30min, stratification, collects upper strata liquid glucose, repeatedly until middle layer is separated out without metaprotein.Liquid glucose 3 times of volume 95% ethanol, 4 DEG C of hold over night, obtain polysaccharide precipitation, and after centrifugal, polysaccharide precipitation 85% ethanol is washed 3 times, vacuum freeze drying obtains polysaccharide, for Selenium Contents.
two, the mensuration of Se content
(1) micro-wave digestion
Accurately take 0.2g(respectively and to be accurate to after radix point four)) test portion or extract the Organic Selenium, selenoprotein and the selenium polysaccharide that obtain, add 5mL HNO
3with 2mL H
2o
2, put into microwave dissolver and carry out micro-wave digestion.After Specimen eliminating completes, be cooled to room temperature, digestion solution be transferred in 100mL volumetric flask, add 1 μ g/mL respectively
72ge and
89in Y is two, mark uses solution 40 μ L, is settled to scale, shakes up with water, to be measured.Micro-wave digestion program is as follows: power 1200W, step 1,120 DEG C, intensification 5min, keeps 5min; Step 2,180 DEG C, intensification 15min, keeps 10min.
(2) blank test
According to the reagent that (one) method process in two contacts with testing sample;
(3) inductivity coupled plasma mass spectrometry measures
Inductivity coupled plasma mass spectrometry condition determination is as follows:
1) RF emissive power: 1.30KW;
2) cooling gas flow: 13.0L/min;
3) atomization gas flow: 0.81L/min;
4) assisted gas flow: 0.78L/min;
5) atomizer: concentric atomizer;
6) spray chamber temperature: 3 DEG C;
7) sampling spiroid/intercepting cone: Nickel;
8) quadrupole rod bias voltage :-13.00 V;
9) sextupole bar bias voltage :-11 V;
10) sampling depth: 120 mm;
11) gas (7%H2:93%He) is collided: 6 mL/min;
12) sampling pattern: entirely quantitative;
13) scan mode: jump peak;
14) integral time: 15 ms;
15) measurement is counted: 3;
16) lifting capacity: 1 mL/min;
17) quality monitoring number: 80.
three, linear relationship and mensuration lower bound
With selenium standard solution Fresh 0,0.2,1,2, the selenium standard working solution of 5,10,20 μ g/L, and make each concentration standard solution all containing 0.40 μ g/L
72ge/
89mark and 5% HNO in Y is two
3.Sample introduction under the determined experiment condition of this law, measures its count value (cps), and with concentration C (μ g/L) for horizontal ordinate, count value (cps) y is ordinate, drawing standard working curve.The standard working curve linear equation of selenium is y=598.57x+27.53, correlation coefficient r=0.9999.
Detecting of this method selenium is limited to 0.006 μ g/L, mensuration lower bound is 3 μ g/kg.
four, the recovery and precision test
In extra large shrimp and sea crab, add the selenium standard solution of three variable concentrations levels respectively, add concentration and be 0.200,5.00,10.0 μ g/L.Recovery scope and precision data are in table 1.
The experimental data of the interpolation concentration of table 1 selenium, recovery scope and RSD
Claims (1)
1. micro-wave digestion-ICP-MS method directly measures the detection method of albumen selenium or polysaccharide selenium in Organic Selenium in marine product, Organic Selenium, it is characterized in that the method comprises the following steps:
One, the preparation of sample
Shelled by sample, all edible part hollanders fully blend and mix, and load sample sack, for subsequent use-18 DEG C of storages, as test portion;
(1) separation and purification of Organic Selenium
Adopt and continue dialysis, accurately take 20.0g test portion and load in bag filter, dialyse 96h in ultrapure water, changes a water every 12h; Test portion after having dialysed is through vacuum freeze drying, for subsequent use-18 DEG C of storages;
(2) separation and purification of selenoprotein
1) accurately take 20.0g test portion in beaker, add 120mL acetone, be placed on magnetic stirring apparatus and stir degreasing 4h, the centrifugal 15min of 8500r/min, abandons supernatant;
2) after volatilizing acetone, add 600mL 0.25mol/L NaOH solution, 50 DEG C of stirring in water bath extract 4h, filter, obtain supernatant;
3) filter residue adds 200mL 0.25mol/L NaOH solution and repeatedly extracts 2 times, merging filtrate, and adding ammonium sulfate to saturation degree is 95%, 4 DEG C of standing 12h;
4) the centrifugal 25min of 8000r/min, precipitates the trishydroxymethylaminomethane-HCl damping fluid with 50mL50mmol/L pH=8.0, dissolves;
5) at 4 DEG C successively with 50mmol/L trishydroxymethylaminomethane-HCl damping fluid, ultrapure water dialysis to BaCl
2solution detects in dislysate without SO
4 2-separate out;
6) test portion after having dialysed through vacuum freeze drying ,-18 DEG C of storages, for Selenium Contents;
(3) separation and purification of selenium polysaccharide
1) Thick many candies extracts: accurately take 20.0g test portion in beaker, after degreasing, add 500mL deionized water, 70 DEG C of water-bath lixiviate 5h, the centrifugal 15min of 8500r/min, collects supernatant; Add 3 times of supernatant volume 95% ethanol, 4 DEG C of hold over night, centrifugal collecting precipitation; Precipitate with deionized water is redissolved, and freeze drying obtains Thick many candies;
2) de-albumen: adopt trypsase+Sevag method to take off albumen, regulate pH to 6.5, add the trypsase of 4% Thick many candies, hatch 6h for 60 DEG C; 100 DEG C of boiling water heating 5min deactivation; Centrifuging and taking supernatant, adds the chloroform-normal butyl alcohol of 1/3 supernatant volume, and the chloroform in chloroform-butanol solution and normal butyl alcohol volume ratio are 4:1, fully rock 30min, stratification, collects upper strata liquid glucose, repeatedly until middle layer is separated out without metaprotein; Liquid glucose 3 times of volume 95% ethanol, 4 DEG C of hold over night, obtain polysaccharide precipitation, and after centrifugal, polysaccharide precipitation 85% ethanol is washed 3 times, vacuum freeze drying obtains polysaccharide, for Selenium Contents;
Two, the mensuration of Se content
(1) micro-wave digestion
Accurately take 0.2g, Organic Selenium, selenoprotein or selenium polysaccharide that test portion or extraction obtain, add 5mL HNO
3with 2mL H
2o
2, put into microwave dissolver and carry out micro-wave digestion, after Specimen eliminating completes, be cooled to room temperature, digestion solution is transferred in 100mL volumetric flask, add 1 μ g/mL
72ge and
89in Y is two, mark uses solution 40 μ L, is settled to scale, shakes up with water, to be measured;
Micro-wave digestion program is as follows: power 1200W, step 1,120 DEG C, intensification 5min, keeps 5min; Step 2,180 DEG C, intensification 15min, keeps 10min;
(2) blank test
According to the reagent that (one) method process in two contacts with testing sample;
(3) inductivity coupled plasma mass spectrometry measures
Inductivity coupled plasma mass spectrometry condition determination is as follows:
1) RF emissive power: 1.30KW;
2) cooling gas flow: 13.0L/min;
3) atomization gas flow: 0.81L/min;
4) assisted gas flow: 0.78L/min;
5) atomizer: concentric atomizer;
6) spray chamber temperature: 3 DEG C;
7) sampling spiroid/intercepting cone: Nickel;
8) quadrupole rod bias voltage :-13.00 V;
9) sextupole bar bias voltage :-11 V;
10) sampling depth: 120 mm;
11) gas is collided: 6 mL/min; Collision gas adopts 7%H
2: 93%He;
12) sampling pattern: entirely quantitative;
13) scan mode: jump peak;
14) integral time: 15 ms;
15) measurement is counted: 3;
16) lifting capacity: 1 mL/min;
17) quality monitoring number: 80.
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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 |
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| CN106596704B (en) * | 2017-02-27 | 2018-12-18 | 山东省食品药品检验研究院 | The method that icp ms measure Se content in vegetables |
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| CN111855834A (en) * | 2020-06-12 | 2020-10-30 | 浙江大学 | Method for measuring total selenium content of selenium-enriched proteoglycan |
| CN111700149A (en) * | 2020-06-29 | 2020-09-25 | 广西壮族自治区农业科学院 | Method for extracting selenium-containing antioxidant active ingredients from purple radix puerariae |
| CN111982874A (en) * | 2020-08-14 | 2020-11-24 | 奥迈检测有限公司 | Method for detecting selenium element in grains |
| CN112649552A (en) * | 2021-01-11 | 2021-04-13 | 南京恒宝田功能农业产业研究院有限公司 | Method for measuring selenium form by using high performance liquid inductively coupled plasma mass spectrometry |
| CN113295762A (en) * | 2021-05-26 | 2021-08-24 | 陕西科技大学 | Method for detecting protein selenium in natural selenium-rich agricultural products |
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