CN114813901A - Method for simultaneously detecting 12 elements in plant sample - Google Patents
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Abstract
The invention discloses a method for simultaneously detecting 12 elements in a plant sample, which relates to the technical field of plant sample analysis and detection, and the technical scheme is characterized in that the method for detecting comprises the following steps: s1, weighing the sample in a microwave digestion inner tank; s2, washing the inner wall of the digestion tank by deionized water, adding the reverse aqua regia digestion solution, covering and placing for 1h, and screwing the tank cover; s3, placing the microwave digestion tank in a microwave digestion instrument for digestion; s4, after the digestion is finished and the plant sample is naturally cooled to room temperature, the cover is unscrewed in a fume hood, and the method has the effects that the plant sample is processed and digested, the aerosol is atomized by an atomizer, the aerosol is converted into charged ion ions in plasma after the steps of dissolution, evaporation, decomposition, ionization and the like, the charged ion ions enter a mass spectrometer, separation and qualitative and quantitative analysis are carried out according to the mass-to-charge ratio of the ions, the content of 12 elements in the plant sample can be detected simultaneously, the operation is simple, and the analysis range is wide.
Description
Technical Field
The invention relates to the technical field of plant sample analysis and detection, in particular to a method for simultaneously detecting 12 elements in a plant sample.
Background
The existing measuring technology for analyzing various elements of plant samples mainly comprises Atomic Absorption Spectrometry (AAS), Atomic Fluorescence Spectrometry (AFS), X-ray fluorescence spectrometry, inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS). Various detection means have advantages and disadvantages, wherein AAS and AFS can only detect specific elements, the analysis accuracy of the X-ray fluorescence spectrometry depends heavily on standard substances, the sensitivity of the X-ray fluorescence spectrometry to ICP-AES with some ultra-low content elements cannot meet the requirement, and the ICP-MS cannot obtain accurate detection results for Se elements with serious mass spectrum interference. The first method of the national standard GB 5009.268-2016 national food safety Standard for the determination of multiple elements in food provides for the determination of inductively coupled plasma mass spectrometry (ICP-MS) of multiple elements in food. However, in actual measurement, due to the existence of mass spectrum interference, the accuracy of analysis is seriously affected, especially for elements such As As, Hg, Se, etc. The content range of each element in the plant sample is wide, the difference is large, and in order to improve the accuracy of sample determination, the determination of the 12 elements in the plant sample can be completed only by multiple times of sample treatment and the determination of multiple high-resolution inductively coupled plasma mass spectrometer devices. Typical matching schemes are: AFS measuring As, Hg and Se; measuring Ni, Cu, Zn and Mn by ICP-AES; and measuring Cr, Cd, Pb, Co and Mo by ICP-MS. In order to improve the analysis performance of multiple elements in plant samples, it is necessary to improve the accuracy and efficiency of analysis. Therefore, there is a need for a simple, fast, accurate and reliable assay for the simultaneous determination of multiple elements in a plant sample.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for simultaneously detecting 12 elements in a plant sample, so as to solve the problems of multiple sample treatments and the measurement of various different devices such as AFS, ICP-AES and ICP-MS in order to improve the accuracy of analysis in the actual production process and improve the efficiency of analysis and measurement.
In order to achieve the purpose, the invention provides the following technical scheme: a method for simultaneously detecting 12 elements in a plant sample, the method having good sensitivity and high accuracy, comprising the steps of:
s1, weighing a proper amount of sample (the sample with lower content or more water content can be properly added with the sampling amount) in the microwave digestion inner tank;
s2, washing the inner wall of the digestion tank by using a small amount of deionized water, adding the reverse aqua regia digestion solution, covering and placing for 1h, and screwing the tank cover;
s3, placing the microwave digestion tank in a microwave digestion instrument for digestion according to the operation steps;
s4, after the digestion is finished and the solution is naturally cooled to room temperature, unscrewing the cover in a fume hood, washing the inner cover with deionized water, transferring the digestion solution into a plastic colorimetric tube, fixing the volume to 50mL with deionized water, shaking up, and standing to obtain a sample solution;
s5, after the high-resolution inductively coupled plasma mass spectrometer is started stably, the high-resolution inductively coupled plasma mass spectrometer is optimized by using standard tuning liquid, so that the high-resolution inductively coupled plasma mass spectrometer meets the detection requirement;
s6, preparing a standard solution and an internal standard solution of each element, taking the concentration of the element to be detected as a horizontal coordinate, taking the ratio of the element to be detected to the response signal value of the selected internal standard element as a vertical coordinate, and establishing a standard curve by using a high-resolution inductively coupled plasma mass spectrometer;
s7, obtaining a detection result according to the standard curve, and converting to obtain the content of various elements in the plant sample, wherein the conversion process is to obtain the concentration of various elements in the plant sample through automatic conversion of the high-resolution inductively coupled plasma mass spectrometer according to the standard curve obtained in S6;
in step S1, if the sample contains ethanol or carbon dioxide, low-temperature heating is required to remove the ethanol or carbon dioxide;
the standard solution and the sample solution in the steps are detected by adopting a high-resolution inductively coupled plasma mass spectrometry technology.
Preferably, the sample is weighed in the step S1 to be 0.2000 g. + -. 0.002g, and the sample amount is increased for the sample with lower content or higher water content.
Preferably, the digestion solution used in step S2 is an aqua regia digestion solution, and the digestion solution is finally determined to be aqua regia by comparing the digestion effects of the digestion systems such as nitric acid, nitric acid-hydrogen peroxide, hydrochloric acid, aqua regia, and aqua regia. Comprehensively, the dosage of the reverse aqua regia is 4 mL.
Preferably, the sample in the step S3 is digested by a microwave digestion instrument, and when the sample is digested, a programmed heating method is generally adopted, the matrix of the plant sample is complex, and the programmed heating can avoid that the reaction of the sample with high organic matter content is too severe, and even a large amount of sample overflows in case of serious reaction. The heating time and temperature should not be too long or too high, otherwise the tube will be softened and accidents will occur. The corresponding working conditions can be adjusted according to the properties of the sample during specific working.
Preferably, the high-resolution inductively coupled plasma mass spectrometer needs to be stabilized for 30min after being started, the high-resolution inductively coupled plasma mass spectrometer is manually tuned by using standard tuning liquid with the mass concentration of 1ng/mL, such as B, Ba, Co, Fe, Ga, In, K, Li, Lu, Na, Rh, Sc, Tl, U, and Y, and the tuned analysis method has the following parameters:
radio frequency power | 1200W | Scanning mode | EScan |
Carrier gas | Ar | Number of scans | 3 |
Flow rate of atomized gas | 1.088L/min | Number of repetitions | 3 |
Flow of cooling gas | 15L/min | Aperture of sampling cone | 1.1mm |
Auxiliary gas flow | 0.8L/min | Diameter of truncated cone | 0.8mm |
Preferably, the standard solution in step S6 is prepared from SPEX mixed standard solution and standard solution of single elements of Hg, Mn, Cu, Zn, etc., and the medium is 8% reverse aqua regia, and the concentration thereof is prepared as follows:
the internal standard solution is prepared from Rh and Ir single element standard solution, and the medium is 2% HNO 3 And the reference concentration of the internal standard solution is 1-5 mug/L.
Preferably, the method for simultaneously detecting 12 elements in the plant sample by using the microwave digestion-high resolution inductively coupled plasma mass spectrometer further comprises a reagent blank, and the reagent blank is prepared by the following method: according to the method of steps S1-S4, reagent blanks can be obtained except for the sample being weighed asymmetrically.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the plant sample detection method, the plant sample is processed and digested, and then atomized into the aerosol through the atomizer, the sample aerosol is converted into ions with charges in the plasma through the steps of dissolving, evaporating, decomposing, ionizing and the like, and then enters the mass spectrometer, separation and qualitative and quantitative analysis are carried out according to the mass-to-charge ratio of the ions, the content of 12 elements in the plant sample can be detected simultaneously, the operation is simple, and the analysis range is wide.
2. Adopt airtight digestion method directly to clear up the plant sample in this application, avoid volatile element's loss, preferably adopt the contrary aqua regia system to carry out the preliminary treatment to the plant sample, the decomposition efficiency is high, and the sample decomposes more thoroughly.
3. The detection method can simultaneously detect 12 elements in the plant sample, the pretreatment process of the sample is simple, the types of the detected elements are multiple, the high-resolution inductively coupled plasma mass spectrometry is adopted to detect the plant sample, the sensitivity is high, the stability is good, the accuracy is high, the detection limit is low, and the simultaneous determination of trace elements and trace elements in the plant sample can be realized.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the following examples are provided to further illustrate the method for simultaneously detecting 12 elements in a plant sample according to the present invention.
The application provides a method for simultaneously detecting 12 elements in a plant sample, which comprises the following steps:
s1, weighing 0.2000g +/-0.002 g of sample (the sample with lower content or more water content can be properly increased in sample amount) in a microwave digestion inner tank, and heating the sample containing ethanol or carbon dioxide on an electric heating plate at low temperature to remove the ethanol or carbon dioxide;
s2, washing the inner wall of the digestion tank by using a small amount of deionized water, adding 4mL of reverse aqua regia digestion solution, covering and placing for 1h, and screwing the tank cover;
s3, placing the microwave digestion tank in a microwave digestion instrument for digestion according to the operation steps;
s4, after the digestion is finished and the solution is naturally cooled to room temperature, unscrewing the cover in a fume hood, washing the inner cover with deionized water, transferring the digestion solution into a plastic colorimetric tube, fixing the volume to 50mL with deionized water, shaking up, and standing to obtain a sample solution;
s5, after the high-resolution inductively coupled plasma mass spectrometer is started and stabilized for 30min, the high-resolution inductively coupled plasma mass spectrometer is optimized by using standard tuning liquid, the optimization process mainly adjusts various parameters of the high-resolution inductively coupled plasma mass spectrometer to enable the high-resolution inductively coupled plasma mass spectrometer to reach the optimal state, the high-resolution inductively coupled plasma mass spectrometer has high sensitivity and stability, the resolution R under medium resolution is more than or equal to 4000, the resolution R under high resolution is more than or equal to 10000, and the detection requirement is met;
s6, preparing multi-element standard solutions with different concentrations, mixing the multi-element standard solutions with an internal standard solution (Rh and Ir solution with the concentration of 1 ng/mL) through a peristaltic pump and a three-way pipe, injecting the mixed solution and the internal standard solution into a high-resolution inductively coupled plasma mass spectrometer, measuring signal response values of elements to be measured and the internal standard element, drawing a standard curve by taking the concentration of the elements to be measured as a horizontal coordinate and the ratio of the response signal values of the elements to be measured and the selected internal standard element as a vertical coordinate, and establishing a standard series curve;
and S7, obtaining a detection result according to the standard curve, and converting to obtain the content of various elements in the plant sample.
Specifically, the source of the high-resolution inductively coupled plasma mass spectrometer device used in the embodiments of the present application: model elemet 2 high resolution inductively coupled plasma mass spectrometer available from Thermo Fisher Scientific, usa; ETHOS UP microwave digestion apparatus from milestone, Italy.
Specifically, the sources of reagents used in the examples of the present application: 100mg/L of the mixed standard solution was purchased from Spex Certiprep, USA; the 1mg/mL single element standard stock solution is purchased from the national analysis and test center for nonferrous metals and electronic materials; 1ng/mL high resolution inductively coupled plasma mass spectrometer tuning solution was purchased from Thermo Fisher Scientific, USA; national primary standards (GBW10010, GBW10014, GBW10015, GBW10020, GBW10048) were purchased from the institute for geophysical geochemistry investigation of the Chinese academy of geology; UP grade nitric acid and hydrochloric acid were purchased from Suzhou Jingrui chemical Co., Ltd; ultrapure water was derived from ultrapure water prepared from an Eckopu AWL-2001-M ultrapure water system (resistivity 18M. omega. cm); a disposable 50mL plastic cuvette was purchased from Thermo Fisher Scientific, USA.
Specifically, in the step S3, the plant sample is pretreated by microwave digestion, which is because microwave digestion has the advantages of high temperature rise, fast heating, strong digestion capability, less acid consumption, low blank value, less volatilization loss and capability of reducing pollution in the sample digestion process. Specific digestion procedures are shown in the following table.
Step (ii) of | Time of temperature rise (min) | Temperature (. degree.C.) | Power (W) |
1 | 15 | 150 | 1800 |
2 | 10 | 160 | 1800 |
3 | 10 | 180 | 1800 |
4 | 5 | 190 | 1800 |
The results obtained with the test method are as follows:
1. selection of isotopes and resolution
When a sample is measured by ICP-MS, non-mass spectrum interference and mass spectrum interference generally exist, most plant samples are complex in matrix, have the characteristics of high salt, high organic matters, high content and the like, and are easy to cause the non-mass spectrum interference to influence the accuracy of an analysis result. Generally, external and internal standard methods can be used for correction of non-mass spectral disturbances. In the experiment, the drift and the matrix effect of the signal are corrected by an internal standard method. For most elements measured in the test, the highest resolution is selected, so that mass spectrum interferences such as polyatomic ion interference, refractory oxide interference and the like can be eliminated. In the analysis work, isotopes with relatively small interference, large abundance and high sensitivity are generally selected for determination. For HR-ICP-MS, high resolution comes at the expense of sensitivity. For known higher levels of elements, high resolution measurements can be used to avoid detector damage from high levels. For some lower element content, a lower mass resolution is conversely selected to ensure higher sensitivity. The table below shows the selection of isotopes and resolutions for the potential interferences of the 12 elements to be measured and the approximate contents of the elements in the sample.
2. Selection of plant sample digestion methods
The dry ashing method uses less reagents and has low blank value, but a sample with a compact structure is not easy to be completely ashed, and partial elements are volatilized and lost at high temperature. The wet digestion sample is completely decomposed, but the reagent consumption is high, and the blank reagent has a large influence on the analysis result. The microwave digestion method also has the problem of large acid consumption, the equipment cost is high, and the complete digestion of the sample can be ensured on the premise of proper acid addition, so that the accuracy and the precision of a detection result are ensured, and the method has the advantages of small acid consumption, low blank value and lower detection limit. Sample pretreatment is performed using microwave digestion.
3. Digestion solution and dosage
A plurality of plant samples are selected for testing, the digestion capacities of digestion systems such as nitric acid, nitric acid-hydrogen peroxide, hydrochloric acid, aqua regia, retrograde aqua regia and the like are compared, and the fact that other digestion solutions except the hydrochloric acid can completely digest the samples is found, so that clear and transparent solutions are obtained. The content of organic matters in a plant sample is very high, the organic matters can be digested by acid with strong oxidizing property, hydrochloric acid cannot completely decompose the organic matters, the digestion capacity of the reverse aqua regia is strong, the determination results of most elements are consistent with the standard values, and the reverse aqua regia system is selected to digest the sample by considering the accuracy of determination of each element. Then, the using amount of the reverse aqua regia is optimized, and 1mL, 2mL, 4mL and 6mL of reverse aqua regia are respectively adopted to digest samples according to the sample digestion process, so that clear and transparent solutions are obtained. But the acidity of the solution is relatively high, and the sample injection system is easily corroded. Therefore, the amount of digestion solution is selected to be 4mL by taking the accuracy and acidity of the measurement into consideration.
4. Standard curve
The standard curves of the elements drawn in the step S6 have correlation coefficients greater than 0.9990, and have good linear relationship, and the regression equation and the correlation coefficients are shown in the following table. Wherein y represents the ratio of the ionic strength of each element to the ionic strength of the internal standard element, and x represents the mass concentration of each element in the solution.
5. Method detection limit
10 sample blank solutions are prepared according to the methods of the steps S1-S4, and are respectively detected, and the sample blank solutions are converted into mass concentration with the unit of ng/g according to a standard curve established by S6. Calculating the standard deviation of the secondary parallel measurement, and calculating the detection limit according to the revised technical guide of environmental monitoring and analysis method Standard (HJ-168): MDL is t (n-1, 0.99) × S, and when n is 10, t is 2.821 with a 4-fold detection limit as a lower measurement limit, and the results are shown in the following table.
6. Precision degree
Digesting the sample according to the method of the steps S1-S4, repeatedly testing the sample for 12 times under the condition of an optimal high-resolution inductively coupled plasma mass spectrometer to obtain the content of each element in the solution, converting the content into mass concentration with the unit of mg/kg, and then respectively calculating the Relative Standard Deviation (RSD) of the content of each element, wherein the results are shown in the following table.
7. Accuracy of
After digesting the samples according to the method of steps S1-S4, we prepared solutions of primary biological standard substances of 5 different countries such as GBW10010, GBW10014, GBW10015, GBW10020, GBW10048, etc., as shown in the following table, the samples were processed and respectively measured 3 times, and then the average value thereof was used as the measured value, the measured results of most of the elements of the samples were matched with the standard value, and as a result, within the uncertainty range, the individual elements of the individual samples have far different measured results due to the uncertainty of the values thereof, and the accuracy of the method is satisfactory, and can meet the measurement requirements of actual samples.
8. Conclusion
In the application, 12 elements such As Cd, Cr, Ni, Cu, Pb, Zn, Co, Mo, As, Hg, Se, Mn and the like in a plant sample are directly measured by HR-ICP-MS after microwave digestion by adopting an inverse aqua regia digestion system, and a simple and rapid plant sample multi-element analysis method is established. The result shows that the mass spectrum interference of multi-atom ions and double-charge ions of the elements to be detected, the signal drift of the high-resolution inductively coupled plasma mass spectrometer and the matrix effect of the sample can be eliminated by selecting the proper resolution and the internal standard elements. The determination result of the national first-level standard substance shows that the method is simple, convenient, stable and reliable, has wide linear range and low detection limit, the precision and the accuracy of the method both meet the analysis requirements on the plant sample in actual determination, the simultaneous determination of trace elements and trace elements in the plant sample is realized, and the method has wide application prospect in the determination of various inorganic elements in the plant sample.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and adaptations to those skilled in the art without departing from the principles of the present invention should also be considered as within the scope of the present invention.
Claims (5)
1. A method for simultaneously detecting 12 elements in a plant sample, the method comprising the steps of:
s1, weighing the sample in a microwave digestion inner tank;
s2, washing the inner wall of the digestion tank by deionized water, adding the reverse aqua regia digestion solution, covering and placing for 1h, and screwing the tank cover;
s3, placing the microwave digestion tank in a microwave digestion instrument for digestion;
s4, after the digestion is finished and the solution is naturally cooled to room temperature, unscrewing the cover in a fume hood, washing the inner cover with deionized water, transferring the digestion solution into a plastic colorimetric tube, fixing the volume to 50mL with deionized water, shaking up, and standing to obtain a sample solution;
s5, after the high-resolution inductively coupled plasma mass spectrometer is started stably, the high-resolution inductively coupled plasma mass spectrometer is optimized by using standard tuning liquid, so that the high-resolution inductively coupled plasma mass spectrometer meets the detection requirement;
s6, preparing a standard solution and an internal standard solution of each element, taking the concentration of the element to be detected as a horizontal coordinate, taking the ratio of the element to be detected to the response signal value of the selected internal standard element as a vertical coordinate, and establishing a standard curve by using a high-resolution inductively coupled plasma mass spectrometer;
s7, obtaining a detection result according to the standard curve, and converting to obtain the content of various elements in the plant sample;
in step S1, if the sample contains ethanol or carbon dioxide, low-temperature heating is required to remove the ethanol or carbon dioxide.
2. The method for simultaneously detecting 12 elements in a plant sample according to claim 1, wherein the sample weighing amount in step S1 is 0.2000g +/-0.002 g, the digestion solution used in step S2 is an aqua regia digestion solution, and the dosage of the aqua regia is 4 mL.
3. The method for simultaneously detecting 12 elements in a plant sample according to claim 1, wherein the sample is digested in step S3 by using a microwave digestion instrument, and the sample is digested by using a programmed heating method.
4. The method of claim 1, wherein the high resolution inductively coupled plasma mass spectrometer is stabilized for 30min after being powered on, and the high resolution inductively coupled plasma mass spectrometer is manually tuned using a standard tuning solution with a mass concentration of 1ng/mL of B, Ba, Co, Fe, Ga, In, K, Li, Lu, Na, Rh, Sc, Tl, U, and Y.
5. The method for simultaneously detecting 12 elements in a plant sample according to claim 1, wherein the standard solution in step S6 is prepared from a SPEX mixed standard solution and a standard solution of single elements of Hg, Mn, Cu, Zn, etc., the medium is 8% reverse aqua regia, the internal standard solution is prepared from a standard solution of single elements of Rh, Ir, the medium is 2% HNO 3 And the reference concentration of the internal standard solution is 1-5 mug/L.
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