CN101813630B - Method for detecting molybdenum element in milk powder - Google Patents
Method for detecting molybdenum element in milk powder Download PDFInfo
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Abstract
The invention relates to a method for detecting molybdenum element in milk powder. The used equipment is an inductively coupled plasma atomic emission spectrometer. The method has the following steps of: 1) preparing molybdenum element standard solution and making a standard curve according to the standard solution; 2) oxidizing a milk powder sample to be tested by using peroxide, performing acid treatment by using nitric acid, digesting in a microwave digestion system, and detecting by using equipment parameters same as the standard solution to obtain a detection result of the sample to be tested; and 3) comparing the detection result of the sample to be tested with the standard curve to determine the content of the molybdenum element in the sample to be tested. The instrument detection limit of the method is 0.0071 mu g/ml, and in an element linear range, the related coefficient r is over 0.999, and the recovery rate is 92.0 to 101.8 percent. The method can quickly and accurately detect the content of the molybdenum element in the milk powder, and has the advantages of low element loss and pollution probability in the sample preparing process, accurate and reliable result, good repeatability and high sensitivity.
Description
Technical field
The present invention relates to the detection method of molybdenum element in a kind of milk powder, particularly a kind of detection method of utilizing the inductively coupled plasma emission spectrometer to measure molybdenum element in the milk powder belongs to the technical field that chemical analysis detects.
Background technology
Molybdenum is the trace element of needed by human.The content of molybdenum is few in human body, and only 1/ten million of percentage of liveweight.Though the content of molybdenum is few, it has very important vital role to people's life.The molybdenum that contains higher proportion in the cardiac muscle of existing known person, molybdenum and some enzymes are being kept the energetic supersession of cardiac muscle jointly.Someone has analyzed the heart of tens examples because of the dead person of miocardial infarction, finds that their the molybdenum amount that contains all is lower than healthy people.This explanation molybdenum directly affects the function of cardiovascular system what of people's in-vivo content, illustrates that also molybdenum has special effect to safeguarding the normal function of heart.
Brainstrust finds that also molybdenum has tangible anticaries action.In the crowd of the area of some scarce molybdenums or molybdenum malabsorption, the incidence of disease of carious tooth is very high among the children, in case after increasing the intake of molybdenum, just can play tangible anticaries action.The someone advises producing and contains molybdenum toothpaste for this reason, to open up the new way of preventing and treating carious tooth.
The adult generally needs the molybdenum of 0.15mg～0.3mg every day.Because molybdenum exists in food more widely, for example all contains molybdenum in the foods such as wheat, beans, milk, eggs, pork and honey, it is extremely low to the requirement of molybdenum to add human body, therefore generally can not lack molybdenum.Some people lacks molybdenum, except the factor that will consider environment or diet, is also noted that absorption and the utilization of human body to molybdenum itself.For example, because of gastrointestinal dysfunction causes the patient who lacks molybdenum, should replenish contain the molybdenum diet in, strengthen diagnosis and treatment to primary disease.Concerning the patient who lacks molybdenum, also there is not real molybdenum class medicine to use at present.So, except changing geographical environment, execute beyond the molydbenum fertilizer, can eat more and contain the abundant food of molybdenum, to improve the content of molybdenum in the human body.
The effect of molybdenum is so important, but so far, the national standard of molybdenum does not also detect in China.We need design the content that the easy method of a cover detects molybdenum element in the milk powder.And the traditional wet manual method of clearing up of general now use detects, and claims sample to add a certain amount of red fuming nitric acid (RFNA) earlier in beaker and spends the night, and adds perchloric acid again to catch up with acid on electric hot plate, repeatedly adds water, dryouies easily in this process, and last acidity also can not be controlled.Add acid and easily other chaff interferences are brought in the sample during water in the process of catching up with acid, sampling amount is many sample will muddy (i.e. incomplete problem be cleared up in existence).Traditional wet manual method of clearing up is not only wasted time and energy, and contaminated environment also has certain injury to the testing staff.
Summary of the invention
The detection method that the purpose of this invention is to provide molybdenum element in a kind of milk powder, this detection method step is simple, linear dependence is good, the result accurately and reliably, and this detection method handling safety, energy savings, environmental protection more.
The invention provides the detection method of molybdenum element in a kind of milk powder, the equipment that this detection method is used is the inductively coupled plasma emission spectrometer, comprises the steps:
1) the molybdenum element standard solution of compound concentration in 0.01 μ g/ml to 2.0 μ g/ml scope, standard solution is carried out the detection of molybdenum element concentration, the typical curve of corresponding relation between the output result of formulation molybdenum element concentration and inductively coupled plasma emission spectrometer;
2) take by weighing the milk powder testing sample, in the milk powder testing sample, add concentration and be 30% hydrogen peroxide and carry out oxidation processes, obtain solution A, in solution A, add concentration and be 65% nitric acid and carry out acid treatment, obtain solution B, place microwave digestion system to clear up solution B, obtain solution C, to solution C use with step 1) in during the standard solution detection identical device parameter carry out the detection of molybdenum element concentration, obtain the testing result of milk powder testing sample;
3) with step 2) in the testing result of milk powder testing sample and the typical curve in the step 1) compare, determine the content of molybdenum element in the milk powder testing sample.
In the detection method of the present invention, used 5% nitric acid to prepare the molybdenum element standard solution in the step 1).
In another embodiment of the present invention, prepared the molybdenum element standard solution of 4 to 8 kinds of variable concentrations in the step 1).
In another kind of embodiment of the present invention, prepared the molybdenum element standard solution of 5 kinds of variable concentrations in the step 1).
In also a kind of embodiment of the present invention, the molybdenum element concentration of standard solution of preparing in the step 1) is respectively 0.05 μ g/ml, 0.1 μ g/ml, 0.5 μ g/ml, 1.0 μ g/ml, 2.0 μ g/ml.
In the detection method of the present invention, step 2) processing procedure of milk powder testing sample comprises the steps: in
21) take by weighing 2.0g to 3.0g milk powder testing sample, put into the teflon digestion tube, add earlier 2ml concentration and be 30% hydrogen peroxide and carry out oxidation, add 4ml concentration again and be 65% nitric acid;
22) with step 21) to handle the solution obtain and put into micro-wave digestion stove micro-wave digestion 51 minutes, the program of micro-wave digestion is as follows:
Power number percent heating-up time min control temperature ℃ retention time min
1600w 100％ 8:00 120 2:00
1600w 100％ 4:00 150 3:00
1600w 100％ 4:00 180 30:00
23) clear up after, take out cooling, it is transferred in the 25ml volumetric flask, be settled to the 25ml mixing with ultrapure water.
In the detection method of the present invention, the hydrogen peroxide that adds in the processing procedure, that nitric acid is top grade is pure.
In the detection method of the present invention, the device parameter of inductively coupled plasma emission spectrometer is as follows: plasma flow amount 15L/min, secondary air amount 0.20L/min, atomizer flow 0.80L/min, sampling volume 1.5ml/min, power 1300W.
In the detection method of the present invention, molybdenum element is adopted axial observation.
The employed superoxol of detection method of the present invention has the effect of oxidation sample, handles sample with it and helps next step sample thoroughly to clear up, and accelerates to clear up speed, and the result who obtains accurately and reliably.Nitric acid solution then makes inorganics and the nitric acid in the solution react, and has reduced the interference of inorganics.The milk powder testing sample by high temperature torch pipe, adopts the multiple-reaction monitoring mode to carry out quantitatively through the atomizing of instrument spray chamber.
This method instrument detects and is limited to 0.0071 μ g/ml, and in the element range of linearity, correlation coefficient r is more than 0.999, and the recovery is 92.0%～101.8% (the interpolation level is 0.25mg/kg, 0.5mg/kg, 1.0mg/kg).
Detection method of the present invention is simple and easy, quick, accurate, and highly sensitive, and its advantage is embodied in following five aspects:
1) method is easy, and particularly the sample preparation process is simple, and element loss and pollution rate are little;
2) linear dependence is good;
3) detect depth of parallelism height, particularly molybdenum element is detected and stablize, parallel result is good;
4) high temperature cabonization, ashing reach wet clearing up for a long time, thereby reach the purpose of energy savings and environmental protection;
5) the sample acidity after handling safety, the ratio of hydrogen peroxide and nitric acid make to be handled can be not too high, avoided to the infringement of instrument with to testing staff's injury.
Generally speaking, method of the present invention is for big-and-middle-sized dairy products enterprise, is the method for molybdenum element in a kind of very practical fast detecting milk powder.
Description of drawings
The following drawings is only done the present invention and is schematically illustrated and explain, not delimit the scope of the invention, wherein:
Fig. 1 is the canonical plotting that is respectively the molybdenum element standard solution formulation of 0.05 μ g/ml, 0.1 μ g/ml, 0.5 μ g/ml, 1.0 μ g/ml, 2.0 μ g/ml according to concentration.
Embodiment
The following stated only is the schematic embodiment of the present invention, is not in order to limit scope of the present invention.Any those skilled in the art, equivalent variations, the modification of being done under the prerequisite that does not break away from design of the present invention and principle and combining all should belong to the scope of protection of the invention.
Embodiment 1
1, the preparation of molybdenum element standard solution
Accurately draw element mark stock solution (concentration 1000 μ g/ml, single mark that national mark affair center is bought), stock solution is diluted with 5% nitric acid, promptly be mixed with the intermediate solution of 10 μ g/ml, prepare the molybdenum element standard solution of variable concentrations again with intermediate solution.Accurately draw intermediate solution by the listed volume of table 1 and place the 50ml volumetric flask, accurately be settled to 50ml with 5% nitric acid, promptly compound concentration is respectively the molybdenum element standard solution of 0.05 μ g/ml, 0.1 μ g/ml, 0.5 μ g/ml, 1.0 μ g/ml, 2.0 μ g/ml.
Required intermediate solution volume (unit: ml) during table 1 preparation molybdenum element standard solution
2, the preparation of 5% nitric acid
Accurately draw 50ml red fuming nitric acid (RFNA) (top grade is pure), place the beaker that the 100ml ultrapure water is arranged approximately, forward to after the cooling in the 1000ml volumetric flask, accurately the constant volume mixing.
3, checkout equipment
The inductively coupled plasma emission spectrometer, the OPtima5300DV inductively coupled plasma emission spectrometer (english abbreviation is ICP-OES) that uses U.S. Perkin-Elmer company to produce.
4, the detection of standard solution
(1) opens main frame and function software, instrument is transferred to optimum condition, open argon gas, water-cooled circulation, preheating four hours.
(2) device parameter of inductively coupled plasma emission spectrometer (being ICP-OES) is: plasma flow amount 15L/min, secondary air amount 0.20L/min, atomizer flow 0.80L/min, sampling volume 1.5ml/min, power 1300W.
(3) concentration of molybdenum element in the detection molybdenum element standard solution, the typical curve of corresponding relation between the output result of formulation molybdenum element concentration and checkout equipment.Typical curve is seen accompanying drawing 1.
5, the processing of testing sample
Take by weighing 2.2718g, 2.2375g, 2.5002g, 2.4896g milk powder testing sample, put into the teflon digestion tube respectively, add earlier 2ml concentration in the sample that takes by weighing and be 30% hydrogen peroxide and carry out oxidation processes, obtain solution A; In solution A, add 4ml concentration then and be 65% nitric acid and carry out acid treatment, obtain solution B; At last, solution B is put into the micro-wave digestion stove carry out micro-wave digestion, the micro-wave digestion program sees the following form 2, clear up 51 minutes after, take out cooling, be transferred in the 25ml volumetric flask, be settled to 25ml with ultrapure water, mixing obtains solution C.
Table 2 micro-wave digestion program
| Power | Number percent | Heating-up time min | Control temperature ℃ | Retention time min |
| 1600w | 100％ | 8:00 | 120 | 2:00 |
| 1600w | 100％ | 4:00 | 150 | 3:00 |
| 1600w | 100％ | 4:00 | 180 | 30:00 |
6, the detection of sample
Do two parallel sample, place porcelain crucible, carry out sample preparation with said method, measure with ICP, molybdenum element is adopted axial observation, device parameter is identical when detecting with standard solution.
Sample message such as input quality, constant volume before sample introduction adopts the multiple-reaction monitoring mode to carry out quantitatively, and promptly multiple element detects simultaneously, and instrument directly calculates the result.After two parallel sample were averaged, testing result saw Table 3:
Table 3 testing result (unit: mg/kg)
To wet a series of processes of resolution method pre-treatment of test sample molybdenum element content of the present invention are simplified to one and a half hours and finish, and have solved wet resolution method when increasing work efficiency greatly and have taken a sample and clear up incomplete problem when too much.The present invention does not have other interference, makes method easier when optimizing link, can also reach the purpose of energy savings and environmental protection.
7, detection limit, the recovery and precision
(1) detection limit is according to 3 times of standard deviation calculation, and method is: with the sample blank duplicate detection, according to the standard deviation that instrument calculates, 3 times of standard deviations are converted into concentration and are detection limit behind the drawing standard curve.As shown in table 4:
The calculating of table 4 detection limit
Detecting in this method solution is limited to 0.0071 μ g/ml.
(2) reclaim experiment to carry out the molybdenum element mark-on with a kind of sample, each recovery test is respectively surveyed three times, draws average recovery rate.It is as shown in table 5 to test concrete data:
The recovery of table 5 sample and precision
(3) through the methodology checking, in the experimental concentration scope, more than the r=0.999, the recovery is between 92.0%～101.8%, shows that this method meets trace element and detects requirement.The RSD of precision experiment is respectively between 1.63%～4.01%.
Embodiment 2
1, the preparation of molybdenum element standard solution
Accurately draw element mark stock solution (concentration 1000 μ g/ml, single mark that national mark affair center is bought), stock solution is diluted with 5% nitric acid, promptly be mixed with the intermediate solution of 10 μ g/ml, prepare the molybdenum element standard solution of variable concentrations again with intermediate solution.Accurately draw intermediate solution by the listed volume of table 6 and place the 50ml volumetric flask, accurately be settled to 50ml with 5% nitric acid, promptly compound concentration is respectively four kinds of variable concentrations molybdenum element standard solution of 0.01 μ g/ml, 0.05 μ g/ml, 0.1 μ g/ml, 0.5 μ g/ml.
Required intermediate solution volume (unit: ml) during table 6 preparation molybdenum element standard solution
2, the preparation of 5% nitric acid
Identical with embodiment 1.
3, checkout equipment
Identical with embodiment 1.
4, standard solution detects
(1) equipment open and preheating identical with embodiment 1.
(2) device parameter is identical with embodiment 1.
(3) concentration of molybdenum element in the detection molybdenum element standard solution, the typical curve of corresponding relation between the output result of formulation molybdenum element concentration and checkout equipment.
5, the processing of testing sample
Take by weighing 2.0008g, 2.3275g, 2.2500g, 2.8649g milk powder testing sample, identical to the processing of milk powder testing sample with embodiment 1.
6, the detection of sample
Do two parallel sample, place porcelain crucible, carry out sample preparation with said method, measure with ICP, molybdenum element is adopted axial observation, device parameter is identical when detecting with standard solution.
Sample message such as input quality, constant volume before sample introduction adopts the multiple-reaction monitoring mode to carry out quantitatively, and promptly multiple element detects simultaneously, and instrument directly calculates the result.After two parallel sample were averaged, testing result saw Table 7:
Table 7 detectable concentration (unit: μ g/ml)
Embodiment 3
1, the preparation of molybdenum element standard solution
Accurately draw element mark stock solution (concentration 1000 μ g/ml, single mark that national mark affair center is bought), stock solution is diluted with 5% nitric acid, promptly be mixed with the intermediate solution of 10 μ g/ml, prepare the molybdenum element standard solution of variable concentrations again with intermediate solution.Accurately draw intermediate solution by the listed volume of table 8 and place the 50ml volumetric flask, accurately be settled to 50ml with 5% nitric acid, promptly compound concentration is respectively eight kinds of variable concentrations molybdenum element standard solution of 0.01 μ g/ml, 0.05 μ g/ml, 0.1 μ g/ml, 0.3 μ g/ml, 0.5 μ g/ml, 1.0 μ g/ml, 1.5 μ g/ml, 2.0 μ g/ml.
Required intermediate solution volume (unit: ml) during table 8 preparation molybdenum element standard solution
2, the preparation of 5% nitric acid
Identical with embodiment 1.
3, checkout equipment
Identical with embodiment 1.
4, standard solution detects
(1) equipment open and preheating identical with embodiment 1.
(2) device parameter is identical with embodiment 1.
(3) concentration of molybdenum element in the detection molybdenum element standard solution, the typical curve of corresponding relation between the output result of formulation molybdenum element concentration and checkout equipment.
5, the processing of testing sample
Take by weighing 2.0588g, 2.3275g, 2.2500g, 3.0002g milk powder testing sample, identical to the processing of milk powder testing sample with embodiment 1.
6, the detection of sample
Do two parallel sample, place porcelain crucible, carry out sample preparation with said method, measure with ICP, molybdenum element is adopted axial observation, device parameter is identical when detecting with standard solution.
Sample message such as input quality, constant volume before sample introduction adopts the multiple-reaction monitoring mode to carry out quantitatively, and promptly multiple element detects simultaneously, and instrument directly calculates the result.After two parallel sample were averaged, testing result saw Table 9:
Table 9 detectable concentration (unit: μ g/ml)
By embodiment 2 and embodiment 3 as can be known, the detectable concentration of sample all is higher than 0.05 μ g/ml (referring to table 7, table 9) in this method, so when preferred embodiment 1 selected molybdenum element concentration of standard solution was respectively 0.05 μ g/ml, 0.1 μ g/ml, 0.5 μ g/ml, 1.0 μ g/ml, 2.0 μ g/ml, typical curve horizontal ordinate lower limit is got 0.05 μ g/ml can satisfy the requirement of test sample to lower limit fully.Molybdenum element does not also add in milk powder at present, and molybdenum more and more is subjected to nutritionists' attention, so be defined in 2.0 μ g/ml on the typical curve horizontal ordinate, not only can satisfy present detection requirement, and also can satisfy the detection requirement when later on molybdenum element content increases.
Above listed a series of detailed description only is specifying at feasibility embodiment of the present invention; they are not in order to restriction protection scope of the present invention, allly do not break away from equivalent embodiment or the change that skill spirit of the present invention done and all should be included within protection scope of the present invention.
Claims (9)
1. the detection method of molybdenum element in the milk powder is characterized in that, the equipment that described detection method is used is the inductively coupled plasma emission spectrometer, and described detection method comprises the steps:
1) the molybdenum element standard solution of compound concentration in 0.01 μ g/ml to 2.0 μ g/ml scope, described standard solution is carried out the detection of molybdenum element concentration, the typical curve of corresponding relation between the output result of formulation molybdenum element concentration and described inductively coupled plasma emission spectrometer;
2) take by weighing 2.0g to 3.0g milk powder testing sample, in described milk powder testing sample, add 2ml concentration and be 30% hydrogen peroxide and carry out oxidation processes, obtain solution A, in described solution A, add 4ml concentration and be 65% nitric acid and carry out acid treatment, obtain solution B, place microwave digestion system to clear up described solution B, obtain solution C, identical device parameter carried out the detection of molybdenum element concentration when described solution C use was detected with standard solution described in the step 1), obtained the testing result of described milk powder testing sample;
3) with step 2) described in typical curve described in the testing result of milk powder testing sample and the step 1) compare, determine the content of molybdenum element in the described milk powder testing sample.
2. detection method as claimed in claim 1 wherein, has used 5% nitric acid to prepare described molybdenum element standard solution in the step 1).
3. detection method as claimed in claim 1 wherein, has been prepared the described molybdenum element standard solution of 4 to 8 kinds of variable concentrations in the step 1).
4. detection method as claimed in claim 3 wherein, has been prepared the described molybdenum element standard solution of 5 kinds of variable concentrations in the step 1).
5. detection method as claimed in claim 4, wherein, the described molybdenum element concentration of standard solution of preparing in the step 1) is respectively 0.05 μ g/ml, 0.1 μ g/ml, 0.5 μ g/ml, 1.0 μ g/ml, 2.0 μ g/ml.
6. the processing procedure of milk powder testing sample comprises the steps: detection method as claimed in claim 1, wherein, step 2)
21) described milk powder testing sample is put into the teflon digestion tube, add described hydrogen peroxide earlier, add described nitric acid again;
22) with step 21) to handle the solution obtain and put into micro-wave digestion stove micro-wave digestion 51 minutes, the program of described micro-wave digestion is as follows:
23) clear up after, take out cooling, it is transferred in the 25ml volumetric flask, be settled to the 25ml mixing with ultrapure water.
7. detection method as claimed in claim 6, wherein, the described hydrogen peroxide that adds in the described processing procedure, that described nitric acid is top grade is pure.
8. detection method as claimed in claim 1, wherein, the described device parameter of described inductively coupled plasma emission spectrometer is as follows: plasma flow amount 15L/min, secondary air amount 0.20L/min, atomizer flow 0.80L/min, sampling volume 1.5ml/min, power 1300W.
9. detection method as claimed in claim 1 wherein, adopts axial observation to described molybdenum element.
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| CN103674671B (en) * | 2012-09-26 | 2015-12-16 | 内蒙古蒙牛乳业（集团）股份有限公司 | A kind ofly detect the pre-treating method of aluminium element in milk powder and use its detection method |
| CN104374628A (en) * | 2013-08-13 | 2015-02-25 | 内蒙古蒙牛乳业（集团）股份有限公司 | Sample pretreatment method of liquid milk metal element detection and detection method using same |
| CN106033072A (en) * | 2015-03-20 | 2016-10-19 | 北京三元食品股份有限公司 | Method for detecting mineral elements in raw milk and dairy products in high throughput mode |
| CN105758812A (en) * | 2016-04-06 | 2016-07-13 | 云南新希望邓川蝶泉乳业有限公司 | Method for rapidly determining lead and chromium in dairy products |
| CN107024464B (en) * | 2017-04-11 | 2019-11-08 | 广西师范大学 | A method of Mo(VI is measured with Surface enhanced Raman spectroscopy) |
| CN112798375B (en) * | 2021-01-06 | 2022-11-22 | 中国海关科学技术研究中心 | Detection device and method for harmful elements in children toothbrush |
| CN115308293A (en) * | 2021-05-08 | 2022-11-08 | 中国石油化工股份有限公司 | Method for measuring molybdenum element in oil product |
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