CN101082627A - Microelement in biological sample and fast analysis method for material - Google Patents
Microelement in biological sample and fast analysis method for material Download PDFInfo
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- CN101082627A CN101082627A CN 200610017858 CN200610017858A CN101082627A CN 101082627 A CN101082627 A CN 101082627A CN 200610017858 CN200610017858 CN 200610017858 CN 200610017858 A CN200610017858 A CN 200610017858A CN 101082627 A CN101082627 A CN 101082627A
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Abstract
The invention discloses a rapid analyzing method of trace element in the biological sample, which comprises the following steps: making the detected sample into solution; plugging the ion selectivity electrode to mate ion analyzer with indexed function or direct read function into the solution; reading the density value of the detected material in the solution; transmitting the density value to the content of element in the sample. The invention makes the paralleling tested RSD% less than 5%, indexed recycling rate over 85% and testing time after dissolving the sample less than 15min, which reduces the cost obviously with error corresponding to blank digestive phase within permitting scale.
Description
Technical field
The invention belongs to the analytical approach of contained trace element and material in the biological sample, relate in particular to the method for express-analysis
Background technology
The mensuration of minor metallic element in the biological sample such as grain, food such as manganese, copper, zinc, iron, lead, cadmium, calcium, magnesium etc., adopt methods such as atomic absorption spectrophotometry, cold-vapour atomic absorption method, atomic fluorescence method and molecule absorption photometric to measure in the national standard method mostly, these methods all need expensive large-scale precision instrument, not only the input cost height also is unfavorable for penetration and promotion and carries out the instant mensuration in scene.
On the other hand, before biological sample is measured, all to clear up sample.Dry ashing commonly used and wet method are cleared up the processing sample.When adopting dry ashing, process required times such as the constant weight of crucible and sample, calcination are very long, and the mensuration of finishing a sample needs 10～12 hours usually, and work efficiency is very low.Adopt wet method to clear up and can produce a large amount of acid vapours, Experimental Establishment has not only been corroded in the volatilization of acid vapor, and severe contamination the environment health that also endangered the operator, therefore this clearing up need be carried out in the fuming cupboard of special use, operation is inconvenience extremely.Wet method is cleared up and is finished the minimum needs 80～100mL of a sample nitration mixture, and minute needs 5～7 hours.
In above-mentioned analytical approach, analysis result need obtain by comparatively complicated calculating or by working curve, not only bothers but also time-consuming in addition.At present, though existing laboratory sample is cleared up special-purpose micro-wave oven product both at home and abroad,, be difficult to promote because of it costs an arm and a leg.
Summary of the invention
It is low to the purpose of this invention is to provide a kind of analysis cost, free from environmental pollution and can measure the analytical approach of trace element and material in the biological sample fast
The present invention seeks to carry out by the following technical programs: the rapid analysis that contains trace element in this biological sample, be earlier determined sample to be made solution to be measured, again the ion-selective electrode that matches with the correction ion analyser with mark-on method function or direct-reading function is well inserted in the solution, from analyser, directly read the concentration value of test substance the tested test solution, then be converted into the content of this element in the analyzed sample.
The method of determined sample being made solution to be measured is, earlier sample is put into container, add acid, will put into after the seal of vessel that micro-wave oven is cleared up or lixiviate 1～40 minute again, then take out in micro-wave oven, the cooling back adds total ion buffering correctives constant volume, mixing.
Determined sample is put into container add acid again, clear up putting into micro-wave oven after the seal of vessel, clear up after 35～40 minutes and in micro-wave oven, take out, cool off and again digestion solution was moved to another container in 4～6 minutes, transferring the pH value of digestion solution is 3～5, then add total ion buffering correctives constant volume, make solution, again the solution after clearing up is poured in the beaker, the ion-selective electrode that matches with the correction ion analyser with mark-on method function or direct-reading function is well inserted in this solution, from analyser, directly read the concentration value of test substance the tested test solution, then be converted into the content of this element in the analyzed sample.
Determined sample is put into container add acid again, take out from micro-wave oven after 1～2 minute putting into the micro-wave oven lixiviate after the seal of vessel, the cooling back adds total ion buffering correctives, the water constant volume is made solution, again the ion-selective electrode that matches with the correction ion analyser with mark-on method function or direct-reading function is well inserted in this solution, from analyser, directly read the concentration value of test substance the tested test solution, then be converted into the content of this element in the analyzed sample.
Described acid is the wherein a kind of of perchloric acid, sulfuric acid, nitric acid, hydrochloric acid, and clearing up is to carry out in the family expenses micro-wave oven.
Described acid is two or three acid mixture in perchloric acid, sulfuric acid, the nitric acid.
The method of determined sample being made solution to be measured is earlier sample to be put into container, adding acid, heat putting into micro-wave oven after the seal of vessel again, add hydrogen peroxide again and be placed in the micro-wave oven and clear up, then take out in micro-wave oven, the cooling back adds total ion buffering correctives constant volume, mixing.
The method of determined sample being made solution to be measured is that elder generation puts into container to sample, adds leaching liquor, container is placed ultrasonic sound appratus lixiviate 2～3 minutes again, then adds total ion buffering correctives constant volume, mixing.
With the method for seal of vessel is with the oral area sealing of teflon seal tape with container, again with the oral area of micro-wave oven special food bag cover bundle at container.
The micro-wave oven of the micro-wave digestion device that adopts among the present invention is general household microwave oven, and is cheap, utilizes this device to clear up sample, the specimen in use amount is few, only uses 0.1～1.0g, and the agent of clearing up that therefore needs is also lacked, the acid mixture consumption only needs 2～9mL, greatly reduces analysis cost; Digestion process is to finish in obturator, and sample is difficult for contaminated, and acid vapour is also free from environmental pollution; Whole digestion process only needs 1～30 minute,
Specimen eliminating finishes, and takes out the back and can be chilled to room temperature being no more than in time of 5 minutes, directly constant volume.Behind the mixing, with proofreading and correct the good ion analyser with mark-on method function or direct-reading function in advance, supporting corresponding ion-selective electrode can directly read the content of tested element, need not mapping and carries out complicated calculations.From sample weighing, clear up pre-service to constant volume, measure until obtaining analysis result etc., The whole analytical process only needs 70-80 minute; If the Specimen eliminating device adopts transparent material to make, the situation of clearing up of sample in can the Direct observation device, be convenient to operation, and utilize this method once can handle the dozens of sample, be applicable to the express-analysis of gross sample, if adopt ultrasonic lixiviate sample, extraction time only needs several minutes, and the The whole analytical process required time is no more than 12 minutes.And the ultrasound wave lixiviate once can be handled the dozens of sample, has improved work efficiency greatly.Mark-on in-line analysis method among the present invention is not only applicable to general sample, is applicable to that also sample complexity or sample form the mensuration of situation such as unclear; Adopt this method, the RSD% of its replicate determination＜5%, recovery of standard addition＞85%, the minute behind the Specimen eliminating＜15 minute, the result is satisfactory.Compare error at measurment within allowed band with blank digestion.
Description of drawings
Fig. 1 is the synoptic diagram after the seal of vessel in the digestion process of the present invention.
Embodiment
Embodiment 1 present embodiment is the fast measuring of micro-cadmium in the wheat flour, and its method and step are:
Take by weighing grey wheat flour 1.0 grams earlier and place the 100mL volumetric flask, add perchloric acid, sulfuric acid acid mixture 9.0mL (wherein the sulfuric acid consumption is 6.0mL, and the perchloric acid consumption is 3.0mL) is capacity bottleneck good seal; The sealing method be to seal its bottleneck with teflin tape, tie bottleneck with micro-wave oven special food bag cover again, the version of good seal as shown in Figure 1,1 is volumetric flask among Fig. 1,2 is teflin tape, 3 is food bag; Cleared up sample and volumetric flask being equipped with, placed household microwave oven, cleared up 37～40 minutes through sealing, clearing up Shi Yingxian cleared up 20 minutes at 40% power shelves, cleared up 17～20 minutes at 60% power shelves again,, be and clear up fully when solution clarification, when transparent, colourless.Take out cooling 5 minutes, solution is transferred in the 50mL beaker, transferring the pH value of solution value is 5, after mixing up, adds total ion buffering correctives, and constant volume, mixing are made solution to be measured.Then the ion-selective electrode that matches with the correction ion analyser with direct-reading method function is well inserted in this solution, and at the uniform velocity stirred 1 minute with magnetic stirring apparatus, draw the concentration value that to measure cadmium element the analyzed sample from analyser, then be converted into the amount that contains cadmium element in the flour.
When measuring the concentration value of contained cadmium element in the above-mentioned solution, concrete operation method can be undertaken by following: under the instrument initial state, entering the concentration mode capabilities by " pattern/4 " key selects, select " 1. direct-reading concentration " by " ▲/0 " or " /" key, by " affirmation " key, the selection that enters concentration unit, still by the different concentration unit of leafing through by " ▲/0 " or " /" key, select " mg/L ", by " affirmation " key.(carried out slope calibration and blank calibration therefore, carried out once more with regard to not needing here).Above-mentioned solution is poured in the 100mL beaker, and the electrode that calibration in advance is good inserts in the solution, and magnetic stirring apparatus at the uniform velocity stirred 1～2 minute, the stable back of potential value on the screen to be shown (generally needing 2～3 minutes), by " affirmation " key, promptly show current concentration value on the instrument, directly read and record.
Instrument should be calibrated before mensuration.
When liquid to be measured prepares, in being housed, the volumetric flask of sample also can only add hydrochloric acid.
Take by weighing grey wheat flour 1.0 grams (being accurate to 0.0001) earlier, place the thin mouthful iodine flask of a 100mL, add sulfuric acid 4.0mL, nitric acid 5.0mL, amount to the acid mixture of 9.0mL, seal bottleneck, tie bottleneck with micro-wave oven special food bag again with teflin tape, place household microwave oven, cleared up 18 minutes earlier, cleared up 17～20 minutes at 60% power shelves again, when the solution that obtains is cleared up fully for clarification, when transparent, colourless at 50% power shelves.Take out cooling 4 minutes, solution is shifted put in the 50mL beaker, transferring the pH value of solution value is 4, is transferred to after mixing up in the 100mL volumetric flask, adds total ion buffering correctives, and constant volume, mixing are made solution to be measured.Again the ion-selective electrode that matches with the correction ion analyser with direct-reading function is well inserted in this solution, drawn the concentration value that to measure copper the analyzed sample, then be converted into the amount that contains copper in the flour from analyser.
The method of operating of the concentration value of mensuration copper is identical with embodiment 1.
When liquid to be measured prepared, in thin mouthful of iodine flask of dress sample, the acid of adding also can be adopted any of nitric acid or sulfuric acid.
The assay method of trace element lead in example 3 wheat flours
Take by weighing about grey wheat flour 1.0 grams (being accurate to 0.0001), place the less resistant to elevated temperatures container of 100mL bore, add nitric acid, sulfuric acid and perchloric acid 9.0mL altogether, their consumption is followed successively by 5mL, 2.5mL and 1.5mL, and with seal of vessel, sealing means is identical with the mode of embodiment 1, then be placed in the Glan scholar household microwave oven, cleared up 20 minutes at 40% power shelves earlier, cleared up 16～19 minutes at 60% power shelves again, when solution clarification, transparent, colourless promptly clearing up fully.Take out cooling 6 minutes, solution is shifted put in the 50mL beaker, transferring the pH value of solution value is 3, is transferred to after mixing up in the 50mL volumetric flask, adds total ion buffering correctives, and constant volume, mixing are made solution to be measured.Again the ion-selective electrode that matches with the correction ion analyser with direct-reading function is well inserted in this solution, and at the uniform velocity stirred 0.5 minute with magnetic stirring apparatus, draw the concentration value that to measure lead element the analyzed sample from analyser, then be converted into and contain the amount of lead element in the powder.
The method of operating of measuring the lead element concentration value is identical with embodiment 1.
When liquid to be measured prepared, in the container of sample was housed, the acid of adding is any in nitric acid, sulfuric acid and the perchloric acid also.
Embodiment 4: present embodiment is a content of measuring micro-fluorine in the feed,
The feed sample 0.5g (accurately to 0.0001g) that took by weighing 40 mesh sieves is in the 50mL volumetric flask, add 5.00mL 1.0mol/LHC1 and 5.00mL water, the teflin tape that cleaned with 6.0mol/LHC1 hydrochloric acid or nitric acid seals bottleneck, place in the Glan scholar household microwave oven with low-grade lixiviate 1～1.5 minute, when the diaphragm seal on placing bottleneck is upwards heaved, take out cooling 2 minutes immediately, take off the band of volumetric flask oral area, wash in bottle with 10mL water, in the washing fluid access capacity bottle, add the total ion buffering of 25.00mL correctives, water constant volume mixing is made solution to be measured.Again the ion-selective electrode that matches with the correction ion analyser with direct-reading function is well inserted in this solution, drawn fluorine element concentration value to be determined the analyzed sample, then be converted into the amount that contains fluorine element in this feed from analyser.
The equipment operation of measuring the lead element concentration value is identical with embodiment 1.
The mensuration of calcium in example 5 wheat flours
Wheat is ground the back sample quarterlies with mortar, at the wheat that takes by weighing 0.25g on the electronic balance (accurately to 0.0001g) in the volumetric flask of 100mL and add the nitric acid of 2.5mL, seal with poly tetrafluoroethylene and bungee, tie bottleneck with micro-wave oven special food bag cover again, then put into micro-wave oven, select 80% power shelves for use, heat repeatedly 3～5 times with micro-wave oven, each 20 seconds, when solution is yellow, with its taking-up, cooled off 1～2 minute, the hydrogen peroxide that adds 2.5mL was again cleared up 40 seconds by above-mentioned identical method and condition, and solution is yellowish transparence, it is taken out from micro-wave oven, be transferred to after the cooling in the 50mL volumetric flask, constant volume, mixing are made solution to be measured.Carry out blank digestion simultaneously.Method by embodiment 1 obtains calcium content in the wheat flour.
Embodiment 6: to the mensuration of trace copper in the wheat
With the method identical 50.00mL solution to be measured is handled and produced to the wheat that will measure, then measure the concentration value of copper in the wheat, be converted into the amount that contains copper in the wheat again with mark-on direct-reading method with embodiment 2.
The method of measuring the concentration of copper in the wheat with mark-on direct-reading method is: the solution 50.00mL to be measured that will produce pours in the beaker, instrument is set input " it is long-pending to add mark liquid " 1.00mL successively, " test liquid volume " 50.00mL, " add and mark liquid concentration " 100mg/L, electrode is inserted in the above-mentioned solution to be measured, behind to be shown the stablizing, by " affirmation " key, then add the long-pending 1.00mL of mark liquid by the volume that configures in advance, concentration, and shake up, after treating that the instrument demonstration is stable, by " affirmation " key, instrument can directly demonstrate copper ion concentration value in the solution to be tested.
Example 7 is the mensuration to the nitrate radical in the wheat flour
Get the wheat flour 1.0g that handles well in the 100mL volumetric flask, add 1.0mol/LNa
2SO
420.00mL in ultrasonic cleaner, with ultrasonic lixiviate 2-3 minute, taking-up was left standstill, and gets supernatant 10mL then, places the 50mL volumetric flask, added 0.0255mol/LAg
2SO
45mL adds 0.5mol/LnaOH, and the pH that transfers above-mentioned solution is 6, uses the redistilled water constant volume again.Then measure the concentration value of nitrate radical in the wheat flour, be converted into the amount that contains nitrate radical in the wheat flour again with mark-on direct-reading method.
Measuring the method that contains nitrate concentration in the wheat flour with mark-on direct-reading method is: the solution to be measured that will produce is poured in the beaker, press instrument prompting input successively " it is long-pending to add mark liquid " 1.00mL then, " test liquid volume " 50.00mL, " add and mark liquid concentration " 100mg/L,, electrode is inserted in the above-mentioned solution by " affirmation " key, behind to be shown the stablizing, by " affirmation " key, then adding concentration is the nitrate radical mark liquid 1.00mL of 100mg/L, shakes up.Behind to be shown the stablizing, by " affirmation " key, instrument just directly provides the concentration value of nitrate radical in the liquid to be measured fast.
In order to be applicable to the express-analysis of gross sample, when sample preparation adopts the ultrasound wave lixiviate among the present invention, once can handle the dozens of sample; Sample preparation adopts once also can handle a plurality of samples when clearing up.Method among the present invention is applicable to cereals such as wheat, corn, beans such as soybean, black soya bean, the mensuration of the component of trace element and suitable leaching liquor in the biological samples such as animal vegetable tissue, fruits and vegetables class, foodstuff.
Claims (9)
1, the rapid analysis that contains trace element in a kind of biological sample, it is characterized in that: earlier determined sample is made solution to be measured, again the ion-selective electrode that matches with the correction ion analyser with mark-on method function or direct-reading function is well inserted in the solution, from analyser, directly read the concentration value of test substance the tested test solution, then be converted into the content of this element in the analyzed sample.
2, rapid analysis according to claim 1, it is characterized in that: the method for determined sample being made solution to be measured is, earlier sample is put into container, add acid, to put into after the seal of vessel that micro-wave oven is cleared up or lixiviate 1～40 minute again, then take out in micro-wave oven, the cooling back adds total ion buffering correctives constant volume, mixing.
3, rapid analysis according to claim 1 and 2, it is characterized in that: determined sample is put into container add acid again, clear up putting into micro-wave oven after the seal of vessel, clear up after 35～40 minutes and in micro-wave oven, take out, cool off and again digestion solution was moved to another container in 4～6 minutes, transferring the pH value of digestion solution is 3～5, then add total ion buffering correctives constant volume, make solution, again the solution after clearing up is poured in the beaker, the ion-selective electrode that matches with the correction ion analyser with mark-on method function or direct-reading function is well inserted in this solution, from analyser, directly read the concentration value of test substance the tested test solution, then be converted into the content of this element in the analyzed sample.
4, rapid analysis according to claim 1 and 2, it is characterized in that: determined sample is put into container add acid again, take out from micro-wave oven after 1～2 minute putting into the micro-wave oven lixiviate after the seal of vessel, the cooling back adds total ion buffering correctives, the water constant volume is made solution, again the ion-selective electrode that matches with the correction ion analyser with mark-on method function or direct-reading function is well inserted in this solution, from analyser, directly read the concentration value of test substance the tested test solution, then be converted into the content of this element in the analyzed sample.
5, rapid analysis according to claim 3: it is characterized in that: described acid is the wherein a kind of of perchloric acid, sulfuric acid, nitric acid, hydrochloric acid, and clearing up is to carry out in the family expenses micro-wave oven.
6, rapid analysis according to claim 3: it is characterized in that: described acid is two or three acid mixture in perchloric acid, sulfuric acid, the nitric acid.
7, rapid analysis according to claim 1, it is characterized in that: the method for determined sample being made solution to be measured is, earlier sample is put into container, add acid, heat putting into micro-wave oven after the seal of vessel again, add hydrogen peroxide again and be placed in the micro-wave oven and clear up, then take out in micro-wave oven, the cooling back adds total ion buffering correctives constant volume, mixing.
8, rapid analysis according to claim 1: it is characterized in that: the method for determined sample being made solution to be measured is, earlier sample is put into container, add leaching liquor, again container is placed ultrasonic sound appratus lixiviate 2～3 minutes, then add total ion buffering correctives constant volume, mixing.
9, rapid analysis according to claim 2: it is characterized in that: with the method for seal of vessel is with the oral area sealing of teflon seal tape with container, again with the oral area of micro-wave oven special food bag cover bundle at container.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111879597A (en) * | 2020-07-20 | 2020-11-03 | 广东石油化工学院 | Buffer solution for detecting nitrate nitrogen in domestic sewage and detection method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111879597A (en) * | 2020-07-20 | 2020-11-03 | 广东石油化工学院 | Buffer solution for detecting nitrate nitrogen in domestic sewage and detection method |
| CN111879597B (en) * | 2020-07-20 | 2023-12-05 | 广东石油化工学院 | Buffer solution for detecting nitrate nitrogen in domestic sewage and detection method |
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