CN106596704A - Method for measuring content of selenium in vegetables through collision cell-inductively coupled plasma source mass spectrometer - Google Patents
Method for measuring content of selenium in vegetables through collision cell-inductively coupled plasma source mass spectrometer Download PDFInfo
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Abstract
The invention relates to a method for measuring the content of selenium in vegetables through collision cell-inductively coupled plasma source mass spectrography. Microwave digestion is used for pretreatment, nitric acid and hydrogen peroxide with oxidability are added, digestion is carried out in a microwave digestion device, a solution obtained after digestion is taken, and an inductively coupled plasma source mass spectrometer is adopted for measurement. The mass number 80 with high abundance is adopted for measuring selenium, a collision cell mode is adopted for the instrument, measuring conditions are improved by adjusting the collision cell voltage and the helium flow, argon interference is reduced, and the precision, accuracy and sensitivity of the measured result are remarkably improved. A sample is pre-treated through microwave digestion, microwaves can penetrate through a digestion tank of polytetrafluoroethylene to heat the sample, and the pressure is high, the digestion speed is high, and the digestion effect is good in the closed digestion tank. The method is simple in process, sensitive, accurate and rapid, and meanwhile is further suitable for measuring selenium in fruits, eggs and other food.
Description
Technical field
The invention belongs to food analyses technical field, is related to a kind of crash response pond-icp mses
The method for determining Se content in vegetable.
Background technology
Selenium is nutrient needed by human, with anticancer, antioxidation, the anti-ageing effect of waiting for a long time, is filled on domestic market
Scold various selenium-enriched foods, but how many contents of selenium specially also needs to us is further gone to determine, so the measure tool of selenium
Significant, the detection of current selenium mainly has hydride generation atomic absorption spectrometry, hydride generation atomic fluorescence method and inductive
ICP-MS, the detection method of selenium is mainly based on hydride generation atomic fluorescence method, but the method is in the mistake of front process
Due to needing the response value of the different valence state for considering selenium different in journey, so in pretreatment process, need to add the potassium ferricyanide,
Hydrochloric acid is repeatedly added, also needs to add hydrochloric acid, potassium hydroxide and potassium borohydride, compared with ICP-MS, experimental implementation when determining
Loaded down with trivial details, finding speed is slow.
Selenium has various isotopes, and the detection that main mass number has 72,74,76,77,78,80,82, element is typically selected
It is measured with the dominant mass number of abundance, because abundance higher employing icp mses are theoretical when determining
Sensitivity is higher, for selenium element,76Se abundance is 9.36%,77Se abundance is 7.63%,78Se abundance is 23.78%,80Se abundance is 49.61%,82 Se abundance is 8.73%.Selenium should be carried out from abundance highest mass number 80 in theory
Determine, but mass number 80 can be interfered during due to being measured using icp mses, due to making
Carrier gas is Ar gas, and the mass number of Ar be 40 determine when with stronger(Ar40+Ar40)80Interference, simultaneously because food
If also there is the calcium of high level, while also existing in product(Ar40+Ca40)80Interference, therefore, existing ICP-MS determine
In the method for selenium, using 80 mass number when detection process all there is the interference that is difficult to eliminate, so previous studies are because skill
Art reason can only adopt other mass numbers such as relatively low other mass numbers such as 78,82 of other abundance, and such as Yin Zhong is " microwave disappears
The technique study of selenium in solution-crash response pool technology inductively coupled plasma mass spectrometry measure grain " and Lv Yuezhen are in " collision
The 78 of selenium mass number is adopted in the articles such as the method that pond inductively coupled plasma mass spectrometry determines Se content in agricultural product "
It is measured, the result for so causing is exactly that sensitivity is relatively low.But78The abundance of Se is 23.60,80The abundance of Se is 49.70,
Use quality number is 80 with higher response value.
Therefore, how to overcome drawbacks described above, set up a kind of simple, sensitive, accurate, the quick and side with higher response value
Method, is current ICP-MS urgent problems in selenium detection application.
The content of the invention
The present invention is for above-mentioned deficiency present in prior art, it is therefore intended that provide a kind of stable and accurate using collision
The method that reaction tank-icp mses determine Se content in vegetable, the inventive method disappear first with microwave
Xie Yi carries out pre-treatment to sample, then using Inductively coupled plasma-mass spectrometry, determines vegetable using collision cell, high helium pattern
The content of middle selenium, can effectively eliminate the interference to selenium when mass number is 80 in detection process, overcome the more low defect of sensitivity.
Technical solution of the present invention is as follows:
The method that a kind of collision cell-icp mses determine Se content in vegetable, step include:
1)Sample pre-treatments:Sample is weighed in politef counteracting tank, nitric acid and hydrogen peroxide is added, in microwave dissolver
Clear up, it is after the completion of clearing up with ultrapure water counteracting tank lid and inwall into politef counteracting tank, then sour electric in catching up with
Hot plate catches up with acid, obtains testing sample solution;
2)Preparing standard solution:Take 10mL concentration be 1000mg/L selenium standard substance in 100mL volumetric flasks, using volume fraction
For 1.5% aqueous solution of nitric acid constant volume, it is then 1~5ng/mL's with the aqueous solution of nitric acid stepwise dilution that volume fraction is 1.5%
Standard solution diluent, it is standby;
3)Draw standard curve:Take the aqueous solution of nitric acid that volume fraction is 1.5% blank as standard solution, and step 2)Match somebody with somebody
The standard solution diluent of system, in the in vitro mass spectrograph such as inductive, using mass number 80, collides pool mode, draws bid
Directrix curve;
4)Sample determination:Step 1)Testing sample solution transfer is settled to 25mL, uses ultra-pure water constant volume, sample to use inductive
Determine etc. in vitro mass spectrograph, using mass number 80, collide pool mode and determine.
Step 1)In, sample is 0.3~0.4g/mL with nitric acid mass volume ratio, and nitric acid is 9 with dioxygen water volume ratio:1.
Step 1)In, micro-wave digestion program is:115 DEG C of holding 9min, 155 DEG C of holding 19min, 185 keep 25min;Work(
Rate is 1600W.
Step 1)In, sour temperature is caught up with for 155 DEG C, the time is 95min.
Step 2)In, the standard solution diluent concentration is 1ng/mL, 2ng/mL, 3ng/mL, 4ng/mL, 5ng/mL
Standard solution diluent.
Further, step 3)With step 4)In, the in vitro mass spectrograph condition determination such as described inductive is:
Time of integration 2s
Internal standard germanium(0.5mg/L)
Helium gas flow 10mL/min
Collision cell entrance potential -130V
Collision cell exit potential -150V.
The beneficial effects of the present invention is:
1. the measure of selenium is carried out using the higher mass number 80 of abundance, and instrument is using collision pool mode, electric by adjusting collision cell
Pressure and helium gas flow reduce argon interference improving condition determination, significantly improve the precision of measurement result, accuracy and
Sensitivity.
2. pre-treatment is carried out using micro-wave digestion to sample, microwave energy penetrates the counteracting tank of politef and sample is carried out
Heating, in closed counteracting tank, pressure is high, and oxidation rate is fast, clears up effect good;
3. procedure is simple, sensitive, accurate, quick, while applying also for the measure of other selenium in food such as fruit, eggs.
Description of the drawings
Fig. 1 is 1 selenium standard curve of embodiment;
Fig. 2 is 1 selenium standard curve of comparative example;
Fig. 3 is 2 selenium standard curve of comparative example.
Specific embodiment
In order that those skilled in the art are better understood from the present invention program, and make the above-mentioned purpose of the present invention, feature
Can become apparent from understandable with advantage, with reference to embodiment, the present invention will be further described in detail.
In the following methods of the present invention, the instrument and equipment and reagent of employing is as follows:
Instrument and equipment:Icp mses(Agilent 7900), microwave dissolver(CEM Mars6), acid it is pure
Change instrument(PerkinElmer).
All glass apparatus soaked overnight in 20% nitric acid, is rinsed repeatedly 6 times with distilled water, finally uses ultra-pure water
Rinse well and dry.
Reagent:Nitric acid(GR), hydrogen peroxide(GR).
Embodiment 1:Choose two kinds of selenium-rich gold needle mushroom samples one, two to be measured
1)Sample pre-treatments:Sample 2.00g is weighed in politef counteracting tank, 9mL nitric acid and 1mL hydrogen peroxide is added, in
Clear up in microwave dissolver, after the completion of clearing up with ultrapure water counteracting tank lid and inwall into politef counteracting tank,
Then in catching up with sour electric hot plate to catch up with acid, obtain testing sample solution;Micro-wave digestion program is:115 DEG C of holding 9min, 155 DEG C of holdings
19min, 185 keep 25min;Power is 1600W.Sour temperature is caught up with for 155 DEG C, the time is 95min;
2)Preparing standard solution:Take 10mL concentration be 1000mg/L selenium standard substance in 100mL volumetric flasks, using volume fraction
For 1.5% aqueous solution of nitric acid constant volume, it is then 1ng/mL, 2ng/ with the aqueous solution of nitric acid stepwise dilution that volume fraction is 1.5%
The standard solution diluent of mL, 3ng/mL, 4ng/mL, 5ng/mL, it is standby;
3)Draw standard curve:Take the aqueous solution of nitric acid that volume fraction is 1.5% blank as standard solution, and step 2)Match somebody with somebody
The standard solution of system draws out standard curve in the in vitro mass spectrograph such as inductive;
4)Sample determination:Step 1)Testing sample solution transfer is settled to 25mL, uses ultra-pure water constant volume, sample to use inductive
Determine etc. in vitro mass spectrograph.
It is to be determined using collision pool mode etc. in vitro mass spectrograph condition determination:
Mass number 80
Time of integration 2s
Internal standard germanium(0.5mg/L)
Helium gas flow is 10mL/min
Collision cell entrance potential -130V
Collision cell exit potential -150V.
Interpretation of result:
Sample one detects that actual Se content is 0.049mg/kg;
Sample two detects that actual Se content is 0.212mg/kg.
Test result indicate that, selenium standard curve(Fig. 1)Linear good R2=0.99907, meet requirement of experiment.
Using embodiment sample one, while being measured to the isotope of the selenium of variable concentrations mass number 78,80,82, survey
Surely the results are shown in Table 1
The isotope assay response value of the selenium of 1 variable concentrations different quality number of table
Measurement result shows that can carry out data analysiss using 80 mass number of the inventive method, 80 mass number response value is substantially high
In other mass numbers.
In embodiment 1, each sample does the mark-on of three different levels, and sample and mark-on are determined 6 times and averaged as most
Final value, assay method ibid, the results are shown in Table 2, table 3:
2 sample of table, one recovery of standard addition measurement result(mg/kg)
3 sample of table, two recovery of standard addition measurement result(mg/kg)
By table 2, table 3 it can be seen that this method to the recovery of standard addition of selenium in vegetable between 96.0%~101.5%,
It is that 3.24%, the 2.89% visible measure selenium under the present embodiment method is sensitive and accurate repeatedly to determine RSD.
Comparative example 1
Differ only in compared with embodiment 1:Collision cell entrance potential -40V, collision cell exit potential -60V.
Determine selenium standard curve and see Fig. 2;
Test result indicate that, the very poor R of selenium standard curve2=0.8778, blank response value is higher, it is impossible to be applied to determination sample.
Test result indicate that, the voltage parameter for changing instrument collision cell can eliminate argon interference, preferably determine vegetable
In selenium, obtain preferable experimental result.
Comparative example 2
The difference compared with embodiment 1 is to adopt Atomic Fluorescence Spectrometry
1)Sample pre-treatments:Sample 2.00g is weighed in politef counteracting tank, 9mL nitric acid and 1mL hydrogen peroxide is added, in
Clear up in microwave dissolver, after the completion of clearing up with ultrapure water counteracting tank lid and inwall into politef counteracting tank,
Then in catching up with sour electric hot plate to catch up with acid near dry, can't be evaporated.5.0mL6mol/L hydrochloric acid solutions are added, continues to be heated to molten
Liquid is changed into Clear colourless and generates with white cigarette, and cooling transfer digestion solution constant volume in 25mL volumetric flasks, mixing are standby, obtain to be measured
Sample solution;
2)Preparing standard solution:Take 10mL concentration be 1000mg/L selenium standard substance in 100mL volumetric flasks, using volume fraction
For 1.5% aqueous solution of nitric acid constant volume, it is then 1ng/mL, 2ng/ with the aqueous solution of nitric acid stepwise dilution that volume fraction is 1.5%
The standard solution diluent of mL, 3ng/mL, 4ng/mL, 5ng/mL, it is standby;
3)Draw standard curve:The standard solution for preparing is taken into 10mL, then salt adding acid 2mL respectively, potassium ferricyanide solution(100g/
L)1.0mL, mixes, makes standard curve, determines in atomic fluorescence spectrometer, draws out standard curve;Condition determination is negative height
Pressure:340V;Lamp current:100mA;Atomization temperature:800℃;Flow rate of carrier gas:500mL/min;Shielding device flow velocity:1000mL/
min;Time delay:1s;Reading duration:15s;Liquid feeding time 8s;Sampling volume:2mL.
4)Sample determination:Step 1)Testing sample solution takes 10mL, then salt adding acid 2mL respectively, potassium ferricyanide solution
(100g/L)1.0mL, mixes, and determines in atomic fluorescence spectrometer, and condition determination is identical with standard curve determination instrument condition.
Bioassay standard curve is shown in Fig. 3;
Each sample does the mark-on of three different levels, and sample and mark-on are determined 6 times and averaged as end value, assay method
Ibid, the results are shown in Table 4, table 5:
4 sample of table, one recovery of standard addition measurement result(mg/kg)
5 sample of table, two recovery of standard addition measurement result(mg/kg)
It is 13.38%, 2.65% that sample repeatedly determines RSD, and the content of atomic Fluorescence Spectrometric Determination of Selenium is that present most domestic is tested
The method that room adopts, by table 4 and table 5 and determine RSD can be seen that in the measure of the selenium of low content atomic fluorescence precision and
Accuracy is not so good as the inventive method, and inventive method obtains good measurement result under variable concentrations level, and at present
The assay method complex operation step that laboratory is adopted mostly, it is higher to experimental skill requirement, increased the not true of experimental result
It is fixed, further demonstrate the practicality of the present invention.
Examples detailed above is not limited by the example for the present invention preferably embodiment, but embodiments of the present invention
System, other any spirit and the changes, modification, replacement made under principle without departing from the present invention, combines, simplifies and be
The substitute mode of effect, is included in protection scope of the present invention.Therefore, protection scope of the present invention should be with claim institute
The protection domain for defining is defined.
Claims (6)
1. the method that a kind of collision cell-icp mses determine Se content in vegetable, it is characterised in that step
Including:
1)Sample pre-treatments:Sample is weighed in politef counteracting tank, nitric acid and hydrogen peroxide is added, in microwave dissolver
Clear up, it is after the completion of clearing up with ultrapure water counteracting tank lid and inwall into politef counteracting tank, then sour electric in catching up with
Hot plate catches up with acid, obtains testing sample solution;
2)Preparing standard solution:Take 10mL concentration be 1000mg/L selenium standard substance in 100mL volumetric flasks, using volume fraction
For 1.5% aqueous solution of nitric acid constant volume, it is then 1~5ng/mL's with the aqueous solution of nitric acid stepwise dilution that volume fraction is 1.5%
Standard solution diluent, it is standby;
3)Draw standard curve:Take the aqueous solution of nitric acid that volume fraction is 1.5% blank as standard solution, and step 2)Match somebody with somebody
The standard solution diluent of system, in the in vitro mass spectrograph such as inductive, using mass number 80, collides pool mode, draws bid
Directrix curve;
4)Sample determination:Step 1)Testing sample solution transfer is settled to 25mL, uses ultra-pure water constant volume, sample to use inductive
Determine etc. in vitro mass spectrograph, using mass number 80, collide pool mode and determine.
2. method according to claim 1, it is characterised in that:Step 1)In, sample and nitric acid mass volume ratio be 0.3~
0.4g/mL, nitric acid are 9 with dioxygen water volume ratio:1.
3. method according to claim 1, it is characterised in that:Step 1)In, micro-wave digestion program is:115 DEG C of holdings
9min, 155 DEG C of holding 19min, 185 keep 25min;Power is 1600W.
4. method according to claim 1, it is characterised in that:Step 1)In, sour temperature is caught up with for 155 DEG C, the time is
95min。
5. method according to claim 1, it is characterised in that:Step 2)In, the standard solution diluent concentration is
The standard solution diluent of 1ng/mL, 2ng/mL, 3ng/mL, 4ng/mL, 5ng/mL.
6. method according to claim 1, it is characterised in that:Step 3)With step 4)In, described inductive etc. is in vitro
Mass spectrograph condition determination is:
Time of integration 2s
Internal standard germanium(0.5mg/L)
Helium gas flow 10mL/min
Collision cell entrance potential -130V
Collision cell exit potential -150V.
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Cited By (6)
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CN110412117A (en) * | 2019-08-24 | 2019-11-05 | 中国水产科学研究院黑龙江水产研究所 | The method that collision cell-inductively coupled plasma mass spectrometry measures 16 kinds of elements in shell simultaneously |
CN111289674A (en) * | 2020-03-10 | 2020-06-16 | 大连市检验检测认证技术服务中心 | Detection method for simultaneously determining five selenium forms in selenium-rich fruits |
CN112630348A (en) * | 2020-12-23 | 2021-04-09 | 河北省地质实验测试中心 | Detection method for detecting selenate selenite in water by using HPLC-ICP-MS |
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 |
CN113720828A (en) * | 2021-09-27 | 2021-11-30 | 江苏省地质工程勘察院 | Method for determining phosphorus and sulfur in fresh plant sample by microwave digestion-ICP-AES (inductively coupled plasma-atomic emission Spectrometry) method |
CN114076793A (en) * | 2020-08-13 | 2022-02-22 | 深圳市疾病预防控制中心(深圳市卫生检验中心、深圳市预防医学研究所) | Method for determining iodine content in food based on inductively coupled plasma mass spectrometry |
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CN110412117A (en) * | 2019-08-24 | 2019-11-05 | 中国水产科学研究院黑龙江水产研究所 | The method that collision cell-inductively coupled plasma mass spectrometry measures 16 kinds of elements in shell simultaneously |
CN111289674A (en) * | 2020-03-10 | 2020-06-16 | 大连市检验检测认证技术服务中心 | Detection method for simultaneously determining five selenium forms in selenium-rich fruits |
CN114076793A (en) * | 2020-08-13 | 2022-02-22 | 深圳市疾病预防控制中心(深圳市卫生检验中心、深圳市预防医学研究所) | Method for determining iodine content in food based on inductively coupled plasma mass spectrometry |
CN114076793B (en) * | 2020-08-13 | 2023-06-09 | 深圳市疾病预防控制中心(深圳市卫生检验中心、深圳市预防医学研究所) | Method for measuring iodine content in food based on inductively coupled plasma mass spectrometry |
CN112630348A (en) * | 2020-12-23 | 2021-04-09 | 河北省地质实验测试中心 | Detection method for detecting selenate selenite in water by using HPLC-ICP-MS |
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 |
CN113720828A (en) * | 2021-09-27 | 2021-11-30 | 江苏省地质工程勘察院 | Method for determining phosphorus and sulfur in fresh plant sample by microwave digestion-ICP-AES (inductively coupled plasma-atomic emission Spectrometry) method |
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