CN104949960A - Method for measuring content of heavy metals in edible mushrooms by ICP-AES (inductively coupled plasma-atomic emission spectrometry) - Google Patents
Method for measuring content of heavy metals in edible mushrooms by ICP-AES (inductively coupled plasma-atomic emission spectrometry) Download PDFInfo
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Abstract
The invention discloses a method for measuring the content of heavy metals in edible mushrooms by ICP-AES (inductively coupled plasma-atomic emission spectrometry), and mainly solves the technical problems that the specific contents of pesticide residues and overproof heavy metals in the edible mushrooms cannot be measured. The method is implemented by the following steps: 1, preparing an experimental material; and 2, pre-treating a sample, preparing a standard solution, measuring working parameters of an instrument, constructing a standard curve and measuring the sample, wherein under the conditions, by adoption of the ICP-AES method, the content of the heavy metals in a mushroom solution is measured; each sample is measured for three times in parallel, and then an average value is calculated; and the contents of all elements in the edible mushrooms can be obtained by carrying out unit conversion on measured data. The measurement method is scientific, accurate, high in measurement precision, quick in measurement and wide in linear range and has the advantages of measuring various elements simultaneously and the like. By the method for measuring harmful substances, poisonous and harmful edible mushrooms can be prevented from entering the market, and the development of an edible mushroom cultivation technology is promoted; and therefore, the method disclosed by the invention has a good popularization prospect.
Description
Technical field:
The present invention relates to the assay method of content of beary metal in a kind of edible fungi, be exactly a kind of method utilizing ICP-AES to measure content of beary metal in edible fungi, belong to species analysis technical field.
Background technology
Since the eighties initial stage, investment is little, the cycle is short, the project of having got rich of instant effect is able to fast development in China as one for edible fungus culturing, and once once supply falls short of demand for edible fungus, and selling price is high.Mushroom industry is a short, adaptable and fast rural economic development project integrating economic benefit, ecological benefits and social benefit, edible fungi is again that a class is organic, nutrition, health care pollution-free food.Compared with other crops, starting is late, the time is short but growth rate is fast, development area is large, so basis is poor, problem is many, and quality and benefits is stable not, and particularly residues of pesticides, harmful heavy metal exceed standard and happen occasionally, Product quality and safety is difficult to effective guarantee, and measures the concrete content of residues of pesticides in edible fungi and heavy metals exceeding standard without reliable method.
Summary of the invention:
The present invention is for the purpose of solving the problem, the technical matters that the residues of pesticides in the edible fungi of mainly solution prior art existence and the concrete content of heavy metals exceeding standard cannot be measured.
For achieving the above object, the present invention adopts following technical proposals: a kind of method utilizing ICP-AES to measure content of beary metal in edible fungi, the method is realized by following step
1 experiment material
1.1 key instruments and running parameter
Adopt DRE inductively coupled plasma atomic emission spectrometer.Power 1.0kW, argon pressure 0.55Mpa, cooling gas flow 15Lmin
-1, atomization gas pressure 379.211kPa, lifting capacity 1.5mLmin
-1, and observation place Automatic Optimal.
Superpure water machine (Airum611di)
Electronic balance (B211D)
1.2 main agents
Nitric acid, hydrogen peroxide
Standard reserving solution: Ni, Cr, Pb, the titer of Cd, As, Hg is 1000 μ gmL
-1country's non-ferrous metal and electronic material Institute of Analysis.
2.1 sample pre-treatments
Edible fungi sample first washs dirt thing with the abluent of 0.15%, and deionized water is cleaned, and then dries to constant weight at 78 DEG C in thermostatic drying chamber, crosses 80 mesh sieve with mortar grinder powdered.Accurately taking sample 0.1000g puts into bottom teflon counteracting tank, adds red fuming nitric acid (RFNA) 3.00mL and 1.00mLH respectively
2o
2, then build inner cap, put into sealable tank, screwing hermetic lid, is then placed in microwave digestion system, and the program arranged according to table 1 is cleared up.After digestion, counteracting tank is cooled to room temperature, pours out digestive juice, is transferred to 25.00mL
-1in volumetric flask, be settled to scale with deionized water, the 3 parts of blank of parallel preparation simultaneously, to be measured.
Table 1 micro-wave digestion sample condition
The preparation of 2.2 standard solution
Mixed standard solution: by 1000 μ gmL
-1standard reserving solution 2% nitric acid stepwise dilution, be mixed to Ni, Cr, Pb, Cd, As, Hg concentration is respectively 0.00,0.10,0.2,0.50,1.00 μ gmL
-1.
2.3 Instrument working parameter
Power 1.0KW, argon pressure 0.55Mpa, cooling gas flow 15Lmin
-1, nebulizer pressure 374.06Pa, lifting capacity 1.5mlmin
-1, observation place Automatic Optimal.
Experimental procedure:
2.4.1 the foundation of typical curve
According to above-mentioned instrument condition, the standard solution of each element 4 concentration point is measured, simultaneously to blank digestion solution ICP-AES method METHOD FOR CONTINUOUS DETERMINATION 10 times, its detection limit (in formula, S sky is the standard deviation of 10 blank solution test concentrations) is calculated by formula D=3S sky, analysis result shows: each elemental standards curve linear related coefficient is all between 0.991 one 0.999, and assay method linear relationship is good
2.4.2 sample tests
Under these conditions, adopt ICP-AES method, carry out assay to the heavy metal in practical fungus solution, every increment product replicate determination 3 times, averages, and the data after mensuration, after unit conversion, can obtain the content of each element in edible fungi.
Beneficial effect of the present invention and feature are: measuring method science, measure accurately and precision of measurement is high, detection limit is low, mensuration is quick, the range of linearity is wide, can the advantage such as Simultaneously test multiple element.By the mensuration of the method to objectionable impurities, stop virulent edible fungi and come into the market, make people eat the edible fungi of nonhazardous relievedly, ensure that people's is healthy, also promote the development of breed of edible fungus technology, therefore, the present invention has good promotion prospect simultaneously.
Embodiment:
Embodiment 1
ICP-AES is utilized to measure a method for content of beary metal in edible fungi, the specific implementation step of the method:
1 experiment material
1.1 key instruments and running parameter
Adopt DRE inductively coupled plasma atomic emission spectrometer (Li Man Leeman company of the U.S.).Power 1.0kW, argon pressure 0.55Mpa, cooling gas flow 15Lmin
-1, atomization gas pressure 379.211kPa, lifting capacity 1.5mLmin
-1, and observation place Automatic Optimal.
Superpure water machine (Airum611di) (German Sai Duolisi).
Electronic balance (B211D) (German Sai Duolisi).
1.2 main agents
Nitric acid, hydrogen peroxide (being top grade pure)
Standard reserving solution: Ni, Cr, Pb, the titer of Cd, As, Hg is 1000 μ gmL
-1country's non-ferrous metal and electronic material Institute of Analysis.
2.1 sample pre-treatments
Mushroom sample is first washed dirt thing with the abluent of 0.15%, and cleans with ionized water, then dry to constant weight at 78 DEG C in thermostatic drying chamber, cross 80 mesh sieve with mortar grinder powdered.Accurately taking sample 0.1000g puts into bottom teflon counteracting tank, adds red fuming nitric acid (RFNA) 3.00mL and 1.00mLH respectively
2o
2, then build inner cap, put into sealable tank, screwing hermetic lid, is then placed in microwave digestion system, and the program arranged according to table 1 is cleared up.After digestion, counteracting tank is cooled to room temperature, pours out digestive juice, is transferred to 25.00mL
-1in volumetric flask, be settled to scale with deionized water, the 3 parts of blank of parallel preparation simultaneously, to be measured.
Table 1 micro-wave digestion sample condition
The preparation of 2.2 standard solution
Mixed standard solution: by 1000 μ gmL
-1standard reserving solution 2% nitric acid stepwise dilution, be mixed to Ni, Cr, Pb, Cd, As, Hg concentration is respectively 0.00,0.10,0.2,0.50,1.00 μ gmL
-1.
2.3 Instrument working parameter
Power 1.0KW, argon pressure 0.55Mpa, cooling gas flow 15Lmin
-1, nebulizer pressure 374.06Pa, lifting capacity 1.5mlmin
-1, observation place Automatic Optimal.
Experimental procedure:
2.4.1 the foundation of typical curve
According to above-mentioned instrument condition, the standard solution of each element 4 concentration point is measured, simultaneously to blank digestion solution ICP-AES method METHOD FOR CONTINUOUS DETERMINATION 10 times, its detection limit (in formula, S sky is the standard deviation of 10 blank solution test concentrations) is calculated by formula D=3S sky, analysis result shows: each elemental standards curve linear related coefficient is all between 0.991 one 0.999, and assay method linear relationship is good
2.4.2 sample tests
Under these conditions, adopt ICP-AES method, carry out assay to the heavy metal in mushroom test sample solution, every increment product replicate determination 3 times, averages, and the data after mensuration, after unit conversion, can obtain the content of each element in edible fungi.
Embodiment 2
ICP-AES is utilized to measure a method for content of beary metal in edible fungi, the specific implementation step of the method:
1 experiment material
1.1 key instruments and running parameter
Adopt DRE inductively coupled plasma atomic emission spectrometer (Li Man Leeman company of the U.S.).Power 1.0kW, argon pressure 0.55Mpa, cooling gas flow 15Lmin
-1, atomization gas pressure 379.211kPa, lifting capacity 1.5mLmin
-1, and observation place Automatic Optimal.
Superpure water machine (Airum611di) (German Sai Duolisi).
Electronic balance (B211D) (German Sai Duolisi).
1.2 main agents
Nitric acid, hydrogen peroxide (being top grade pure)
Standard reserving solution: Ni, Cr, Pb, the titer of Cd, As, Hg is 1000 μ gmL
-1country's non-ferrous metal and electronic material Institute of Analysis.
2.1 sample pre-treatments
Coprinus comatus sample is first washed dirt thing with the abluent of 0.2%, and cleans with ionized water, then dry to constant weight at 78 DEG C in thermostatic drying chamber, cross 80 mesh sieve with mortar grinder powdered.Accurately taking sample 0.1000g puts into bottom teflon counteracting tank, adds red fuming nitric acid (RFNA) 3.00mL and 1.00mLH respectively
2o
2, then build inner cap, put into sealable tank, screwing hermetic lid, is then placed in microwave digestion system, and the program arranged according to table 1 is cleared up.After digestion, counteracting tank is cooled to room temperature, pours out digestive juice, is transferred to 25.00mL
-1in volumetric flask, be settled to scale with deionized water, the 3 parts of blank of parallel preparation simultaneously, to be measured.
Table 1 micro-wave digestion sample condition
The preparation of 2.2 standard solution
Mixed standard solution: by 1000 μ gmL
-1standard reserving solution 2% nitric acid stepwise dilution, be mixed to Ni, Cr, Pb, Cd, As, Hg concentration is respectively 0.00,0.10,0.2,0.50,1.00 μ gmL
-1.
2.3 Instrument working parameter
Power 1.0KW, argon pressure 0.55Mpa, cooling gas flow 15Lmin
-1, nebulizer pressure 374.06Pa, lifting capacity 1.5mlmin
-1, observation place Automatic Optimal.
Experimental procedure:
2.4.1 the foundation of typical curve
According to above-mentioned instrument condition, the standard solution of each element 4 concentration point is measured, simultaneously to blank digestion solution ICP-AES method METHOD FOR CONTINUOUS DETERMINATION 10 times, its detection limit (in formula, S sky is the standard deviation of 10 blank solution test concentrations) is calculated by formula D=3S sky, analysis result shows: each elemental standards curve linear related coefficient is all between 0.991 one 0.999, and assay method linear relationship is good
2.4.2 sample tests
Under these conditions, adopt ICP-AES method, carry out assay to the heavy metal in coprinus comatus test sample solution, every increment product replicate determination 3 times, averages, and the data after mensuration, after unit conversion, can obtain the content of each element in edible fungi.
Except above-mentioned mushroom, coprinus comatus, the present invention is also suitable for the mensuration to other edible fungi Pesticides and content of beary metal, as: the mensuration of flat mushroom, HUAZIGU, asparagus, pleurotus eryngii, agrocybe, White mushroom, black fungus and Cordceps militaris etc.
Claims (3)
1. utilize ICP-AES to measure a method for content of beary metal in edible fungi, the method is realized by following step:
1 experiment material
1.1 key instruments and running parameter
Adopt DRE inductively coupled plasma atomic emission spectrometer, power 1.0kW, argon pressure 0.55Mpa, cooling gas flow 15Lmin
-1, atomization gas pressure 379.211kPa, lifting capacity 1.5mLmin
-1, and observation place Automatic Optimal, Superpure water machine (Airum611di), electronic balance (B211D);
1.2 main agents
Nitric acid, hydrogen peroxide
Standard reserving solution: Ni, Cr, Pb, the titer of Cd, As, Hg is 1000 μ gmL
-1country's non-ferrous metal and electronic material Institute of Analysis;
2.1 sample pre-treatments
Edible fungi sample first washs dirt thing with the abluent of 0.15%, deionized water is cleaned, then dry to constant weight at 78 DEG C in thermostatic drying chamber, 80 mesh sieve are crossed with mortar grinder powdered, accurately taking sample 0.1000g puts into bottom teflon counteracting tank, adds red fuming nitric acid (RFNA) 3.00mL and 1.00mLH respectively
2o
2, then build inner cap, put into sealable tank, screwing hermetic lid, is then placed in microwave digestion system, and the program arranged according to table 1 is cleared up, and after digestion, counteracting tank is cooled to room temperature, pours out digestive juice, is transferred to 25.00mL
-1in volumetric flask, be settled to scale with deionized water, the 3 parts of blank of parallel preparation simultaneously, to be measured;
Table 1 micro-wave digestion sample condition
The preparation of 2.2 standard solution
Mixed standard solution: by 1000 μ gmL
-1standard reserving solution 2% nitric acid stepwise dilution, be mixed to Ni, Cr, Pb, Cd, As, Hg concentration is respectively 0.00,0.10,0.2,0.50,1.00 μ gmL
-1;
2.3 Instrument working parameter
Power 1.0KW, argon pressure 0.55Mpa, cooling gas flow 15Lmin
-1, nebulizer pressure 374.06Pa, lifting capacity 1.5mlmin
-1, observation place Automatic Optimal, experimental procedure:
2.4.1 the foundation of typical curve
According to above-mentioned instrument condition, the standard solution of each element 4 concentration point is measured, simultaneously to blank digestion solution ICP-AES method METHOD FOR CONTINUOUS DETERMINATION 10 times, its detection limit is calculated by formula D=3S sky, analysis result shows: each elemental standards curve linear related coefficient is all between 0.991 one 0.999, and assay method linear relationship is good;
2.4.2 sample tests
Under these conditions, adopt ICP-AES method, carry out assay to the heavy metal in practical fungus solution, every increment product replicate determination 3 times, averages, and the data after mensuration, after unit conversion, can obtain the content of each element in edible fungi.
2. a kind of method utilizing ICP-AES to measure content of beary metal in edible fungi according to claim 1, the practical fungus in the method adopts mushroom, and its sample first washs dirt thing with the abluent of 0.15%.
3. a kind of method utilizing ICP-AES to measure content of beary metal in edible fungi according to claim 1, the practical fungus in the method adopts coprinus comatus, and its sample first washs dirt thing with the abluent of 0.2%.
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| CN107764801A (en) * | 2016-08-20 | 2018-03-06 | 江西三和金业有限公司 | A kind of method that stable measure scraps graphite crucible residue gold |
| CN108489967A (en) * | 2018-03-26 | 2018-09-04 | 四川大学 | A kind of micro- spectral method traced to the source for phoenix tail chicken |
| CN109799228A (en) * | 2019-03-21 | 2019-05-24 | 利尔化学股份有限公司 | Utilize the method for palladium element residual quantity in ICP-OES method measurement pinoxaden product |
| CN110186909A (en) * | 2019-06-20 | 2019-08-30 | 上海瀚海检测技术股份有限公司 | Heavy metal element in micro-wave digestion and ICP-OES test leather and fur products |
| CN113358455A (en) * | 2021-05-13 | 2021-09-07 | 沈阳市食品药品检验所 | Method for automatically and rapidly digesting food sample |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105606392A (en) * | 2016-02-16 | 2016-05-25 | 上海屹尧仪器科技发展有限公司 | Full-automatic microwave pretreatment method |
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| CN109799228A (en) * | 2019-03-21 | 2019-05-24 | 利尔化学股份有限公司 | Utilize the method for palladium element residual quantity in ICP-OES method measurement pinoxaden product |
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| CN113358455A (en) * | 2021-05-13 | 2021-09-07 | 沈阳市食品药品检验所 | Method for automatically and rapidly digesting food sample |
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Application publication date: 20150930 |