CN117723624A - Method for simultaneously detecting contents of various heavy metal elements in Phellinus linteus - Google Patents
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- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 52
- 241000001727 Tropicoporus linteus Species 0.000 title claims abstract description 41
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Abstract
The invention provides a method for simultaneously detecting contents of various heavy metal elements in Phellinus linteus, belonging to the technical field of heavy metal element detection; the method comprises the steps of sample solution preparation, heavy metal standard solution preparation, sample determination, calculation of the content of various heavy metal elements and the like, and can sensitively and accurately detect the content of various heavy metal elements in the Phellinus linteus; in addition, the method selects the element which does not generate mass spectrum interference to the element to be detected 103 Rh as a single internal standard element reduces non-mass spectral interference from physical effects and matrix effects; by adding to mixed standard working solutionsThe Au element is used as a mercury stabilizer to prevent non-mass spectrum interference of memory effect; using HNO 3 As the unique digestion reagent, the reagent dosage is small, the digestion effect is good, the interference of non-metallic element mass spectrum and other pollution are not easy to be introduced, and the addition of H into the mulberry Huang Yangpin in the microwave digestion process is avoided 2 O 2 A large amount of foam is generated to adhere to the inner wall of the digestion tube.
Description
Technical Field
The invention belongs to the technical field of heavy metal element detection, and particularly relates to a method for simultaneously detecting contents of various heavy metal elements in Phellinus linteus.
Background
Inductively coupled plasma mass spectrometry (ICP-MS) is an inorganic element and isotope analysis test technology developed in the 80 s of the 20 th century, which combines the high-temperature ionization characteristics of inductively coupled plasma with the advantage of sensitive rapid scanning of a mass spectrometer by a unique interface technology to form a high-sensitivity analysis technology; the plasma used by the ICP-MS instrument is substantially the same as that used in the emission spectrum except for the orientation and coil grounding; the mass analyzer, ion detector and data acquisition system used are again similar to quadrupole GC-MS instruments; the mass analyzer adopts a quadrupole mass spectrometer, and also adopts a double-focusing sector magnetic field mass spectrometer with high resolution, a time-of-flight mass spectrometer and the like; the technology is characterized in that: the sensitivity is high, the speed is high, and the quantitative determination of tens of elements can be completed in a few minutes; the spectral line is simple, and the interference is less than that of the spectral technique; the linear range can reach 7-9 orders of magnitude; the preparation and introduction of the sample are simple compared with other mass spectrometry technologies; the method can be used for elemental analysis and rapid determination of isotope composition; the measurement precision (RSD) can reach 0.1 percent; the heavy metal elements can irreversibly deform protein, lose physiological activity, have certain carcinogenicity, and accumulate in human bodies to cause long-term harm, so that the accurate determination of the heavy metal elements in Phellinus linteus is a key technology for evaluating the safety of Phellinus linteus;
GB 5009.268-2016 (determination of multiple elements in food) and SN/T0448-2011 (detection method of arsenic, mercury, lead and cadmium in import and export food) both adopt an inductively coupled plasma mass spectrometer as an analysis instrument, and a sample treatment method for microwave digestion is also provided, so that multiple heavy metal elements can be detected simultaneously, but the methods are all general standards for food detection;
at present, no technical method for detecting the content of heavy metal elements in Phellinus linteus fruiting bodies and decoction pieces exists, only some analysis methods of heavy metal elements in foods and Chinese medicinal materials can be used for reference, and most of the methods detect single elements by adopting an atomic fluorescence or atomic absorption method, are complex and cumbersome to operate, have large reagent dosage and are not suitable for multi-element simultaneous rapid analysis; meanwhile, the detection methods are all general methods, the characteristics of Phellinus linteus cannot be detected, and because Phellinus linteus is flocculent after being crushed, the sample weighing amount, the use and the use amount of reagents are considered, in addition, the content levels of different elements in Phellinus linteus are considered, and the solution after digestion is optimized for volume fixing, insoluble substance treatment, standard solution linear range, internal standard element use, mercury stabilizer selection, proportion and the like; the method for detecting heavy metal elements in Phellinus linteus by using inductively coupled plasma mass spectrometer is suitable for simultaneously detecting the content of various heavy metal elements in Phellinus linteus, but there is still non-mass spectrum interference from physical effect, matrix effect and memory effect; in addition, microwave digestion of organic samples typically employs HNO with low interference 3 -H2O 2 System, but Phellinus Linteus sample is added with H 2 O 2 A large amount of foam is generated and attached to the inner wall of the digestion tube, which is a technical problem to be solved.
Disclosure of Invention
Aiming at the technical method for detecting the heavy metal element content in Phellinus linteus fruiting bodies and decoction pieces in the prior art, the method for detecting single element by adopting atomic fluorescence or atomic absorption is complex and cumbersome in operation, large in reagent dosage, not suitable for rapid analysis of multiple elements at the same time, and does not accord with the characteristics of Phellinus linteus; therefore, the method for simultaneously detecting the contents of various heavy metal elements in the Phellinus linteus comprises the steps of sample solution preparation, heavy metal standard solution preparation, sample determination, calculation of the contents of various heavy metal elements and the like, and can sensitively and accurately detect the contents of various heavy metal elements in the Phellinus linteus simultaneously.
In order to achieve the above purpose, the technical scheme adopted in the application is as follows:
a method for simultaneously detecting contents of various heavy metal elements in Phellinus linteus comprises the following specific steps:
step one: sample solution preparation: weighing a Phellinus linteus sample 0.2000-g which is dried and crushed into coarse powder, putting the Phellinus linteus sample in a microwave digestion tank, adding 8-mL nitric acid solution, uniformly mixing, covering and standing for more than 30 min, putting the Phellinus linteus sample in a microwave digestion instrument for microwave digestion, taking out the Phellinus linteus sample after cooling, flushing an inner cover with a small amount of pure water, heating at 120 ℃ to remove acid until the residual content is 1-2 mL, cooling, transferring the Phellinus linteus sample to a container, and standing until the pure water is constant to 25 mL;
step two: preparing a heavy metal standard solution: preparing a series of standard solutions containing Au, wherein the concentrations of the standard solutions are respectively 0, 10, 20, 50, 100 and 200 mug/L; preparing a series of standard solutions containing Cr, wherein the concentrations of the standard solutions are respectively 0, 10, 20, 50, 100 and 200 mug/L; preparing a series of standard solutions containing Cu, wherein the concentrations of the standard solutions are respectively 0, 5, 10, 25, 50 and 100 mug/L; preparing a series of standard solutions containing Pb, wherein the concentrations of the standard solutions are respectively 0, 2.5, 5, 12.5, 25 and 50 mug/L; preparing a series of standard solutions containing As, wherein the concentrations of the standard solutions are respectively 0, 0.5, 1, 2.5, 5 and 10 mug/L; preparing a series of standard solutions containing Cd, wherein the concentrations of the standard solutions are respectively 0, 0.5, 1, 2.5, 5 and 10 mug/L; preparing a series of standard solutions containing Hg, wherein the concentrations are respectively 0, 0.1, 0.2, 0.5, 1 and 2 mug/L; meanwhile, rh solution with the concentration of 20 mug/L is also prepared as an internal standard solution;
step three: sample measurement: tuning the inductively coupled plasma mass spectrometer to an optimal operating state; sequentially injecting mixed standard working solution into an inductively coupled plasma mass spectrometer from low concentration to high concentration, synchronously adding an internal standard solution on line by the instrument, measuring response signals of the element to be measured and the internal standard element, drawing an internal standard method calibration curve by taking the ratio of the response signal value of the element to be measured and the internal standard element in the standard solution as an ordinate and the concentration of the element to be measured as an abscissa; sequentially injecting the whole-program blank solution and the sample solution to be tested into an instrument, and obtaining the concentration of the element to be tested in the sample solution to be tested through a calibration curve after deducting the signal value of the whole-program blank;
step four: calculating the content of each heavy metal element: calculating the content of heavy metals in the liquid to be measured by the following formula: x= (C-C) 0 ) X V/(M x 1000), where: the symbol X is the content of heavy metal in the liquid to be detected, and the unit is milligrams per kilogram (mg/kg); symbol C is the concentration of heavy metal in the liquid to be detected, and the unit is micrograms per liter (mug/L); symbol C 0 Concentration of heavy metals in the blank solution is expressed in micrograms per liter (mug/L); the symbol V is the volume of the liquid to be measured, and the unit is milliliter (mL); the symbol M is the sampling amount of the liquid to be measured, and the unit is gram (g).
Preferably, in the first step, the mass fraction of nitric acid added into the microwave digestion tank is 65%.
Preferably, in the first step, the microwave digestion procedure is as follows: in a microwave digestion instrument, setting a target temperature at 120 ℃ for 5 min, and then preserving heat for 5 min; setting a target temperature, heating to 150 ℃ for 5 min, and then preserving heat for 10 min; finally, setting a target temperature of 190 ℃ and heating for 5 min, and then preserving heat for 20 min.
Preferably, in the second step, the specific operation of preparing the heavy metal standard solution is as follows: preparing an element stock solution, and preparing a unit element stock solution by a mass method by taking a nitric acid solution (1+49) As a medium, wherein the concentration of Cr, cu and Pb stock solutions is 10000 mug/L, and the concentration of As, cd and Hg stock solutions is 100 mug/L; meanwhile, preparing mercury stabilizing solution: weighing 0.5 g of Au element standard solution to 50 g by using nitric acid solution (1+49); finally, preparing a mixed standard working solution: the mercury stabilizer series working solutions are prepared by taking a certain mass of each element stock solution and mercury stabilizer and gradually diluting the stock solution and the mercury stabilizer by a nitric acid solution (1+49) by a mass method.
Preferably, in the third step, selecting 52 Cr、 63 Cu、 75 As、 114 Cd、 202 Hg as the mass number of Cr, cu, as, cd, hg element and Pb element 206 Pb、 207 Pb、 208 The sum of Pb is the test object; 6 heavy metal elements to be detected 103 Rh is an internal standard element; wherein, 75 As、 114 correcting interference of the isobaric element by Cd through an interference correction equation; as ofThe interference correction equation is: [ 75 As]= [75]-3.127×([77]-0.815×[82]) The method comprises the steps of carrying out a first treatment on the surface of the The interference correction equation for Cd is [ 114 Cd]= [114]-0.0268×[118]。
Compared with the prior art, the invention has the advantages and positive effects that:
1. the method for simultaneously detecting the contents of various heavy metal elements in the Phellinus linteus comprises the steps of sample solution preparation, heavy metal standard solution preparation, sample determination, calculation of the contents of various heavy metal elements and the like, and can sensitively and accurately detect the contents of various heavy metal elements in the Phellinus linteus simultaneously;
2. the non-mass spectrum interference of ICP-MS detection comes from physical effect and matrix effect, the internal standard method is used for correcting the most common effective measure for reducing the matrix effect and instrument fluctuation, the internal standard should select the element which is not in the sample and has stable property, the element which is similar to the mass number and ionization energy of the element to be detected is usually preferentially considered, but the research considers that the two are unnecessary conditions, the element which is not in the sample should be preferentially selected, and the internal standard element does not produce mass spectrum interference to the element to be detected, the method selects 103 Rh is used as a single internal standard element;
3. memory effect belongs to non-mass spectrum interference of ICP-MS, and Hg element can be strongly adsorbed in a container and a sample injection system, so that memory effect is generated, the Hg content in a standard solution and a sample solution is unstable, and the flushing time of sample analysis is increased; the Au and Hg can form stable gold amalgam, so that the memory effect is reduced, and the Au element is added into the mixed standard working solution to serve as a mercury stabilizer, wherein the mass ratio of the Au element to the Hg is 100:1;
4. microwave digestion of organic samples typically employs less interfering HNO 3 -H 2 O 2 System, but Phellinus Linteus sample is added with H 2 O 2 After that, a large amount of foam is generated and attached to the inner wall of the digestion tube, and HNO is used in the method 3 As a unique digestion reagent, the consumption of the reagent is small, the digestion effect is good, and the interference of non-metallic element mass spectrum and other pollution are not easy to introduce.
Detailed Description
In order that the above objects, features and advantages of the invention may be more clearly understood, a further description of the invention will be provided with reference to the following examples. It should be noted that, in the case of no conflict, the embodiments of the present application and the features in the embodiments may be combined with each other.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, however, the present invention may be practiced otherwise than as described herein, and therefore the present invention is not limited to the specific embodiments of the disclosure that follow.
Embodiment 1, a method for simultaneously detecting contents of various heavy metal elements in Phellinus linteus, specifically comprises the following steps:
step one: sample solution preparation: weighing 0.2. 0.2 g (accurate to 0.0001 g) of the Phellinus linteus sample dried and crushed into coarse powder, adding 8 mL mass percent of 65% nitric acid solution into a microwave digestion tank, uniformly mixing, covering and standing for more than 30 min, and then placing into a microwave digestion instrument for microwave digestion, wherein the microwave digestion procedure is shown in Table 1; after the microwave digestion is finished, cooling, taking out, flushing the inner cover with a small amount of pure water, heating at 120 ℃ to remove acid until the residual acid is 1 mL, cooling, transferring to a container, fixing the volume of the pure water to 25 mL, and standing to remove insoluble impurities;
table 1 microwave digestion procedure
Step two: preparing a heavy metal standard solution:
preparing an element stock solution, and preparing a unit element stock solution by a mass method by taking a nitric acid solution (1+49) As a medium, wherein the concentration of Cr, cu and Pb stock solutions is 10000 mug/L, and the concentration of As, cd and Hg stock solutions is 100 mug/L;
meanwhile, preparing mercury stabilizing solution: weighing 0.5 g of Au element standard solution to 50 g by using nitric acid solution (1+49);
finally, preparing a mixed standard working solution: taking a certain mass of each element stock solution and mercury stabilizer, and gradually diluting the stock solution and the mercury stabilizer by a nitric acid solution (1+49) by a mass method to prepare a series of working solutions containing the mercury stabilizer: preparing a series of standard solutions containing Au, wherein the concentrations of the standard solutions are respectively 0, 10, 20, 50, 100 and 200 mug/L; preparing a series of standard solutions containing Cr, wherein the concentrations of the standard solutions are respectively 0, 10, 20, 50, 100 and 200 mug/L; preparing a series of standard solutions containing Cu, wherein the concentrations of the standard solutions are respectively 0, 5, 10, 25, 50 and 100 mug/L; preparing a series of standard solutions containing Pb, wherein the concentrations of the standard solutions are respectively 0, 2.5, 5, 12.5, 25 and 50 mug/L; preparing a series of standard solutions containing As, wherein the concentrations of the standard solutions are respectively 0, 0.5, 1, 2.5, 5 and 10 mug/L; preparing a series of standard solutions containing Cd, wherein the concentrations of the standard solutions are respectively 0, 0.5, 1, 2.5, 5 and 10 mug/L; preparing a series of standard solutions containing Hg, wherein the concentrations are respectively 0, 0.1, 0.2, 0.5, 1 and 2 mug/L; meanwhile, rh solution with the concentration of 20 mug/L is also prepared as an internal standard solution;
step three: sample measurement: tuning the inductively coupled plasma mass spectrometer to an optimal operating state; selecting 52 Cr、 63 Cu、 75 As、 114 Cd、 202 Hg is taken as a test object of Cr, cu, as, cd, hg element, and Pb element 206 Pb、 207 Pb、 208 The sum of Pb is the test object; 6 heavy metal elements to be detected 103 Rh is an internal standard element; wherein the method comprises the steps of 75 As、 114 Correcting interference of the isobaric element by Cd through an interference correction equation; the interference correction equation for As is: [ 75 As]= [75]-3.127×( [77]-0.815×[82]) The method comprises the steps of carrying out a first treatment on the surface of the The interference correction equation for Cd is [ 114 Cd]= [114]-0.0268×[118]The method comprises the steps of carrying out a first treatment on the surface of the Sequentially injecting mixed standard working solution into an inductively coupled plasma mass spectrometer from low concentration to high concentration, synchronously adding an internal standard solution on line by the instrument, measuring response signals of the element to be measured and the internal standard element, drawing an internal standard method calibration curve by taking the ratio of the response signal value of the element to be measured and the internal standard element in the standard solution as an ordinate and the concentration of the element to be measured as an abscissa; sequentially injecting the whole-program blank solution and the sample solution to be tested into an instrument, and obtaining the concentration of the element to be tested in the sample solution to be tested through a calibration curve after deducting the signal value of the whole-program blank;
step four: calculating the content of each heavy metal element: calculating the content of heavy metals in the liquid to be measured by the following formula:X＝(C-C 0 ) X V/(M x 1000), where: the symbol X is the content of heavy metal in the liquid to be detected, and the unit is milligrams per kilogram (mg/kg); symbol C is the concentration of heavy metal in the liquid to be detected, and the unit is micrograms per liter (mug/L); symbol C 0 Concentration of heavy metals in the blank solution is expressed in micrograms per liter (mug/L); the symbol V is the volume of the liquid to be measured, and the unit is milliliter (mL); the symbol M is the sampling amount of the liquid to be measured, the unit is gram (g), the results are shown in Table 2,
TABLE 2 heavy metal contents in Phellinus linteus samples
The results of example 1 were then subjected to method verification:
(1) calibration curve and method detection limit: drawing an internal standard calibration curve equation, continuously measuring a blank solution of the whole procedure of an experiment for 11 times, converting the mass concentration of each element to be detected in the solution into mass fraction, calculating standard deviation S, detecting limit MDL=3S by the method, reserving 1-bit effective number, and only entering nothing, wherein the conc represents the concentration of the element to be detected, and the [ I/S Ratio ] represents the recovery rate of the internal standard. The correlation coefficient of the linear regression equation of the 6 heavy metal elements is not lower than 0.999, and the detection limit of the method is between 0.00009 mg/kg and 0.0009 mg/kg;
TABLE 3 calibration Curve equation and method detection limits
(2) Repeatability and recovery: 6 Phellinus linteus samples are prepared in parallel for testing, the average value and RSD of the content of each element are calculated, and the repeatability of the method is verified; accurately weighing the sample 0.200 and g, respectively adding 2 groups of mixed standard solutions with different concentration levels according to the content level of each element in the sample, preparing 6 parts of mixed standard solutions with each concentration level in parallel, testing the content of the element after the addition of the standard, taking the average value of the content of each element in the measured sample as a background, and calculating the recovery rate. The repeatability and recovery rate results are shown in Table 4, the RSD (relative standard deviation) of the content measurement of 6 heavy metal elements in the sample is between 1.79% and 7.26%, and the standard average recovery rate is between 89.3% and 107.5%.
Table 4 method repeatability and recovery test (n=6)
(3) Standard substance determination: the astragalus standard substance GSB-19 is selected to verify the applicability and the result accuracy of the method, 6 parts of the method are prepared in parallel for testing, the average measured value and the RSD are calculated, and the result is shown in Table 5; the content of the test elements in the standard substance is within the standard value range, and the RSD is between 1.54% and 6.04%.
Table 5 standard substance measurement results (n=6)
The present invention is not limited to the above-mentioned embodiments, and any equivalent embodiments which can be changed or modified by the technical content disclosed above can be applied to other fields, but any simple modification, equivalent changes and modification made to the above-mentioned embodiments according to the technical substance of the present invention will still fall within the protection scope of the technical solution of the present invention.
Claims (5)
1. A method for simultaneously detecting contents of various heavy metal elements in Phellinus linteus is characterized by comprising the following specific steps:
step one: sample solution preparation: weighing a Phellinus linteus sample 0.2000-g which is dried and crushed into coarse powder, putting the Phellinus linteus sample in a microwave digestion tank, adding 8-mL nitric acid solution, uniformly mixing, covering and standing for more than 30 min, putting the Phellinus linteus sample in a microwave digestion instrument for microwave digestion, taking out the Phellinus linteus sample after cooling, flushing an inner cover with a small amount of pure water, heating at 120 ℃ to remove acid until the residual content is 1-2 mL, cooling, transferring the Phellinus linteus sample to a container, and standing until the pure water is constant to 25 mL;
step two: preparing a heavy metal standard solution: preparing a series of standard solutions containing Au, wherein the concentrations of the standard solutions are respectively 0, 10, 20, 50, 100 and 200 mug/L; preparing a series of standard solutions containing Cr, wherein the concentrations of the standard solutions are respectively 0, 10, 20, 50, 100 and 200 mug/L; preparing a series of standard solutions containing Cu, wherein the concentrations of the standard solutions are respectively 0, 5, 10, 25, 50 and 100 mug/L; preparing a series of standard solutions containing Pb, wherein the concentrations of the standard solutions are respectively 0, 2.5, 5, 12.5, 25 and 50 mug/L; preparing a series of standard solutions containing As, wherein the concentrations of the standard solutions are respectively 0, 0.5, 1, 2.5, 5 and 10 mug/L; preparing a series of standard solutions containing Cd, wherein the concentrations of the standard solutions are respectively 0, 0.5, 1, 2.5, 5 and 10 mug/L; preparing a series of standard solutions containing Hg, wherein the concentrations are respectively 0, 0.1, 0.2, 0.5, 1 and 2 mug/L; meanwhile, rh solution with the concentration of 20 mug/L is also prepared as an internal standard solution;
step three: sample measurement: tuning the inductively coupled plasma mass spectrometer to an optimal operating state; sequentially injecting mixed standard working solution into an inductively coupled plasma mass spectrometer from low concentration to high concentration, synchronously adding an internal standard solution on line by the instrument, measuring response signals of the element to be measured and the internal standard element, drawing an internal standard method calibration curve by taking the ratio of the response signal value of the element to be measured and the internal standard element in the standard solution as an ordinate and the concentration of the element to be measured as an abscissa; sequentially injecting the whole-program blank solution and the sample solution to be tested into an instrument, and obtaining the concentration of the element to be tested in the sample solution to be tested through a calibration curve after deducting the signal value of the whole-program blank;
step four: calculating the content of each heavy metal element: calculating the content of heavy metals in the liquid to be measured by the following formula: x= (C-C) 0 ) X V/(M x 1000), where: the symbol X is the content of heavy metal in the liquid to be detected, and the unit is milligrams per kilogram (mg/kg); symbol C is the concentration of heavy metal in the liquid to be detected, and the unit is micrograms per liter (mug/L); symbol C 0 Concentration of heavy metals in the blank solution is expressed in micrograms per liter (mug/L); the symbol V is the volume of the liquid to be measured, and the unit is milliliter (mL); the symbol M is the sampling amount of the liquid to be measured, and the unit is gram (g).
2. The method for simultaneously detecting contents of a plurality of heavy metal elements in Phellinus linteus according to claim 1, wherein in the first step, the mass fraction of nitric acid added into the microwave digestion tank is 65%.
3. The method for simultaneously detecting contents of a plurality of heavy metal elements in Phellinus linteus according to claim 1, wherein in the first step, the microwave digestion procedure is as follows: in a microwave digestion instrument, setting a target temperature at 120 ℃ for 5 min, and then preserving heat for 5 min; setting a target temperature, heating to 150 ℃ for 5 min, and then preserving heat for 10 min; finally, setting a target temperature of 190 ℃ and heating for 5 min, and then preserving heat for 20 min.
4. The method for simultaneously detecting contents of a plurality of heavy metal elements in Phellinus linteus according to claim 1, wherein in the second step, the specific operation of preparing the heavy metal standard solution is as follows: preparing an element stock solution, and preparing a unit element stock solution by a mass method by taking a nitric acid solution (1+49) As a medium, wherein the concentration of Cr, cu and Pb stock solutions is 10000 mug/L, and the concentration of As, cd and Hg stock solutions is 100 mug/L; meanwhile, preparing mercury stabilizing solution: weighing 0.5 g of Au element standard solution to 50 g by using nitric acid solution (1+49); finally, preparing a mixed standard working solution: the mercury stabilizer series working solutions are prepared by taking a certain mass of each element stock solution and mercury stabilizer and gradually diluting the stock solution and the mercury stabilizer by a nitric acid solution (1+49) by a mass method.
5. The method for simultaneously detecting contents of a plurality of heavy metal elements in Phellinus linteus as set forth in claim 1, wherein in the third step, selecting 52 Cr、 63 Cu、 75 As、 114 Cd、 202 Hg is taken as a test object of Cr, cu, as, cd, hg element, and Pb element 206 Pb、 207 Pb、 208 The sum of Pb is the test object; 6 heavy metal elements to be detected 103 Rh is an internal standard element.
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