Method for determining four heavy metal elements in artificial tiger bone powder by inductively coupled plasma mass spectrometry

Abstract

The invention relates to a method for determining four heavy metal elements in artificial tiger bone powder through inductively coupled plasma mass spectrometry, and belongs to the technical field of traditional Chinese medicine detection. The determination method comprises the following steps: (1) preparing a solution: preparing a lead, arsenic and cadmium stock solution 1; preparing a lead, arsenic and cadmium stock solution 2; preparing a copper stock solution 1; preparing an internal standard solution; (2) preparing a test solution; (3) content determination: pumping the test solution and the internal standard solution into an atomizer by using a peristaltic pump by adopting an online internal standard method, mixing, and determining in an inductively coupled plasma mass spectrometer; (4) drawing a standard curve: respectively and precisely measuring proper amounts of lead, arsenic and cadmium stock solutions 2 and copper stock solution 1, preparing a series of linear relation investigation solutions with concentrations, and carrying out linear regression by taking the concentrations as abscissas and the response values as ordinates. According to the method, the detection of the heavy metal elements in the artificial tiger bone powder is optimally designed.

Description

Technical Field

[0001] The present application relates to the technical field of traditional Chinese medicine detection, and in particular to a method for determining four heavy metal elements in artificial tiger bone powder by inductively coupled plasma mass spectrometry. Background Art

[0002] In the existing technical field, the detection methods for the four heavy metals arsenic (As), cadmium (Cd), copper (Cu) and lead (Pb) in artificial tiger bone powder are mainly atomic absorption method and atomic fluorescence hydride method. The complex matrix components in the sample may lead to the enhancement or weakening of the absorption signal, affecting the accuracy of the measurement results, and it is impossible to measure multiple elements at the same time, and the analysis cycle is long. With the country's increasing attention to drug quality and safety in recent years, how to ensure the safety of people's medication while meeting everyone's medication needs has become a major problem faced by artificial tiger bone powder in the production and inspection process.

[0003] Because heavy metal elements are significantly toxic and may cause chronic harm to human health even at low concentrations, the control of heavy metal elements is an indispensable part of drug quality control and is directly related to the safety, effectiveness and health of drugs. In order to accurately determine the content of heavy metal elements arsenic (As), cadmium (Cd), copper (Cu) and lead (Pb) in artificial tiger bone powder, it is necessary to establish an efficient, accurate and sensitive analytical method. This requires a series of technical breakthroughs, including the optimization of sample pretreatment methods, the selection and calibration of analytical instruments, and the establishment of data analysis methods. Through technical breakthroughs, the accuracy and sensitivity of the analysis can be improved, and errors and interferences can be reduced. It not only helps to evaluate the safety and effectiveness of artificial tiger bone powder and provide a scientific basis for clinical medication, but also promotes the development and innovation of quality control technology for Chinese herbal medicines. Summary of the invention

[0004] In view of this, the present application provides a method for determining four heavy metal elements in artificial tiger bone powder by inductively coupled plasma mass spectrometry. The method of the present application is optimized and designed for the detection of heavy metal elements in artificial tiger bone powder, and a new method for the detection of heavy metal elements in artificial tiger bone powder is established. The sample pretreatment steps in the traditional detection method are simplified, making the detection process more intuitive and easy to understand, and improving the detection efficiency, which can effectively overcome the defects of the above-mentioned prior art.

[0005] The present application provides a method for determining four heavy metal elements in artificial tiger bone powder by inductively coupled plasma mass spectrometry, comprising the following steps:

[0006] (1) Preparation of solution:

[0007] Preparation of lead, arsenic and cadmium stock solution 1: put lead single element solution standard substance, arsenic single element solution standard substance and cadmium single element solution standard substance into the same volumetric flask, dilute to scale with solvent, and shake well to obtain lead, arsenic and cadmium stock solution 1;

[0008] Preparation of lead, arsenic and cadmium stock solution 2: take lead, arsenic and cadmium stock solution 1 and place it in a volumetric flask, dilute to the mark with solvent, and shake well to obtain lead, arsenic and cadmium stock solution 2;

[0009] Preparation of copper stock solution 1: Place copper single element solution standard substance in a volumetric flask, dilute to scale with solvent, and shake well to obtain copper stock solution 1;

[0010] Preparation of internal standard solution: Accurately pipette Bi, Ge and In multi-element standard solutions into a volumetric flask, add solvent to make up to the mark, and shake well to obtain a mixed internal standard solution of Bi, Ge and In;

[0011] (2) Preparation of test solution: accurately weigh the test sample and place it in a digestion tube, add nitric acid, and place it overnight. Before digestion, add hydrogen peroxide solution, cover and tighten, place in a microwave digestion instrument for digestion, remove the digestion tube after digestion is complete, place it in an acid remover to remove acid, remove it and let it cool, transfer the liquid in the digestion tube to a volumetric flask, dilute to the mark with ultrapure water, shake well, filter with a microporous filter membrane, and take the filtrate;

[0012] (3) Content determination: The online internal standard method is used to pump the test solution and the internal standard solution into the nebulizer using a peristaltic pump and then mix them into the inductively coupled plasma mass spectrometer for determination;

[0013] (4) Plotting of standard curve: Accurately measure appropriate amounts of lead, arsenic, cadmium stock solution 2 and copper stock solution 1, respectively, to prepare a series of concentration linear relationship test solutions, and perform linear regression with concentration as the horizontal axis and response value as the vertical axis.

[0014] This application is specially designed for the determination of the content of heavy metal elements arsenic (As), cadmium (Cd), copper (Cu) and lead (Pb) in artificial tiger bone powder, and has significant technical advantages. This application can effectively determine the content of heavy metal elements arsenic (As), cadmium (Cd), copper (Cu) and lead (Pb) in artificial tiger bone powder, ensuring the quality and safety of artificial tiger bone powder. Compared with the traditional statutory method, this application scheme can quickly and simultaneously determine multiple heavy metal elements, greatly shortening the overall operation steps of the original method. The defects of cumbersome, repetitive, time-consuming and labor-intensive, and most importantly, the sample preparation process is simple and fast, greatly improving the detection efficiency, reducing the uncertainty factors caused by human operation, and ensuring the accuracy and reliability of the data. This series of characteristics makes this application scheme an ideal choice for the detection of heavy metal elements arsenic (As), cadmium (Cd), copper (Cu) and lead (Pb) in artificial tiger bone powder. It not only simplifies the laboratory operation process, but also provides technical support and reference basis for the quality control, safety evaluation and product development of artificial tiger bone powder.

[0015] Preferably, in step (3), the isotopes selected for determination are 208Pb, 75As, 114Cd and 63Cu, wherein 208Pb uses 209Bi as an internal standard, 114Cd uses 115In as an internal standard, and 75As and 63Cu use 72Ge as an internal standard.

[0016] Preferably, in step (2), the usage ratio of the test sample, nitric acid and hydrogen peroxide solution is 0.1 g:8 ml:1 ml.

[0017] Preferably, in step (2), the mass fraction of the hydrogen peroxide solution is 30%.

[0018] Preferably, in step (2), the acid removal temperature is 80° C. and the acid removal time is 30 minutes.

[0019] Preferably, in step (2), the pore size of the filter membrane is 0.22 μm.

[0020] Preferably, in step (1), the solvent is a 10% nitric acid solution, and the preparation process of the 10% nitric acid solution is as follows: take 100 ml of nitric acid, add ultrapure water to dilute to 1000 ml, and obtain a 10% nitric acid solution.

[0021] Preferably, in step (1), the lead concentration in the lead, arsenic and cadmium stock solution 1 is 10 μg / ml, the arsenic concentration is 10 μg / ml, and the cadmium concentration is 5 μg / ml.

[0022] Preferably, in step (1), the lead concentration in the lead, arsenic and cadmium stock solution 2 is 1000 ng / ml, the arsenic concentration is 1000 ng / ml, and the cadmium concentration is 500 ng / ml.

[0023] Preferably, in step (1), the concentration of the copper stock solution 1 is 10 μg / ml; or

[0024] In step (1), the concentration of the mixed internal standard solution of Bi, Ge and In is 500 ng / ml.

[0025] Compared with the prior art, this application has the following beneficial effects:

[0026] 1. High sensitivity and low detection limit: ICP-MS technology has extremely high sensitivity and low detection limit, and can detect trace levels of heavy metal elements. This high sensitivity enables ICP-MS to accurately detect low levels of heavy metals in artificial tiger bone powder, meeting strict quality control and safety standards.

[0027] 2. Simultaneous determination of multiple elements: ICP-MS can simultaneously determine multiple heavy metal elements, greatly improving the analysis efficiency. Compared with the traditional single element analysis method, ICP-MS can simultaneously detect As, Cd, Cu and Pb in one analysis process, reducing sample processing and analysis time and improving work efficiency.

[0028] 3. Good linear range and accuracy: ICP-MS shows good linearity in the determination of heavy metals, with correlation coefficients usually greater than 0.999; at the same time, verification has shown that this method has high accuracy and precision.

[0029] 4. Rapid analysis capability: ICP-MS has a fast analysis speed and can complete multi-element determination of samples in a short time, which is of great significance for scenarios that require rapid testing of a large number of samples (such as quality control of artificial tiger bone powder).

[0030] 5. Strong anti-interference ability: ICP-MS can effectively overcome the interference of matrix effect and signal drift through the internal standard method and optimized digestion conditions; for example, in the detection of human samples, the matrix effect is corrected by adding internal standard elements (such as Bi, Ge, In), ensuring the reliability of the test results.

[0031] 6. The new ICP-MS method for determining heavy metals in artificial tiger bone powder in this application has the advantages of high sensitivity, low detection limit, simultaneous determination of multiple elements, good linear range and accuracy, etc., and can meet strict quality control and safety testing requirements; it not only helps to evaluate the safety and effectiveness of artificial tiger bone powder and provide a scientific basis for clinical medication, but also promotes the development and innovation of quality control technology for Chinese medicinal materials; by continuously developing and optimizing technology to meet the needs of the market and consumers, it will bring tangible benefits to pharmaceutical companies, health product manufacturers, scientific research institutions and consumers; at the same time, government departments and enterprises should also strengthen cooperation to jointly promote the normalization, standardization and scientific development of the Chinese medicinal materials market. DETAILED DESCRIPTION

[0032] In order to make the purpose, technical solution and advantages of this application clearer, the technical solution in this application will be described clearly and completely below. Obviously, the described embodiments are part of the embodiments of this application, not all of them. Based on the embodiments in this application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of this application.

[0033] The detection method of this application is the standard curve method.

[0034] 1. Instruments, equipment and reagents information

[0035] 1.1 Instruments and Equipment

[0036] Inductively coupled plasma mass spectrometer Agilent 7800.

[0037] 1.2 Reagent Information

[0038] As shown in Table 1.

[0039] Table 1 Reagent information

[0040]

[0041] 2 Methods and Results

[0042] 2.1 Instrument parameters

[0043] The analysis conditions were tuning mode #1He; RF power 1600w; RF match 1.40V; sampling depth 10.0mm; nebulizer gas 0.34L / min; peristaltic pump 0.10rps; nebulizer chamber temperature 2℃; extraction lens 2 was -195.0V; Ome ga deflection voltage -80V; Ome ga lens 11.2V; collision cell inlet -40V; collision cell outlet -60V; Deflect 1.6V; Plate Bias-55V; helium flow rate 5ml / min; octopole deflection voltage -18.0V; octopole RF200V; energy discrimination 5.0V.

[0044] 2.2 Solution preparation

[0045] Solvent: 10% nitric acid solution (Take 100ml of nitric acid and dilute it to 1000ml with ultrapure water.

[0046] Lead, arsenic, and cadmium stock solutions 1: Take 1 ml of lead single element solution standard substance, 1 ml of arsenic single element solution standard substance, and 0.5 ml of cadmium single element solution standard substance and place them in the same 100 ml volumetric flask, dilute to the mark with 10% nitric acid solution, and shake well to obtain a lead concentration of 10 μg / ml, an arsenic concentration of 10 μg / ml, and a cadmium concentration of 5 μg / ml.

[0047] Lead, arsenic, and cadmium stock solution 2: Take 5 ml of lead, arsenic, and cadmium stock solution 1 and place it in a 50 ml volumetric flask, dilute to the mark with 10% nitric acid solution, and shake well to obtain a lead concentration of 1000 ng / ml, an arsenic concentration of 1000 ng / ml, and a cadmium concentration of 500 ng / ml.

[0048] Copper stock solution 1: Take 1 ml of copper single element solution standard substance and place it in a 100 ml volumetric flask, dilute to the mark with 10% nitric acid solution, and shake well to obtain a concentration of 10 μg / ml.

[0049] The preparation of the standard curve is shown in Table 2.

[0050] Table 2 Preparation of standard curve

[0051]

[0052] The above preparations are all diluted to 100 ml volumetric flasks with 10% nitric acid solution.

[0053] Preparation of internal standard solution:

[0054] Accurately pipette 5 ml of Bi, Ge, In multi-element standard solution into a 100 ml volumetric flask, add 10% nitric acid solution to the scale, shake well, and you will get a mixed internal standard solution containing 500 ng / ml of Bi, Ge, and In. During the entire measurement process, the internal standard solution is pumped into the instrument at a constant speed of 0.1 r / min through a peristaltic pump.

[0055] Preparation of test solution:

[0056] Take about 0.1g of the sample, weigh it accurately, put it in a 50ml digestion tube, add 8ml of nitric acid, leave it overnight, add 1ml of 30% hydrogen peroxide solution before digestion, cover and tighten, and place it in MARS6 microwave digestion instrument for digestion. The microwave digestion conditions are detailed in Table 3. After the digestion is complete, remove the digestion tube and place it on an acid remover at 80℃ for 30 minutes, take it out, and let it cool. Carefully transfer the liquid in the digestion tube to a 100ml volumetric flask, dilute to the scale with ultrapure water and shake well. Filter with a microporous filter membrane (0.22μm) and take the filtrate.

[0057] Take an empty 50ml digestion tube, add 8ml nitric acid, place overnight, add 1ml 30% hydrogen peroxide solution before digestion, cover and tighten, place in MARS6 microwave digestion instrument for digestion, microwave digestion conditions are detailed in Table 3, after digestion is complete, remove the digestion tube and place in an acid remover at 80℃ for 30 minutes, take out, and cool. Carefully transfer the liquid in the digestion tube to a 100ml volumetric flask, dilute to the scale with ultrapure water and shake well. Filter with a microporous filter membrane (0.22μm), and take the filtrate to obtain the reagent blank solution.

[0058] The reagent blank solution can determine the impurities or background signals that may exist in the reagents and solvents, so that they can be deducted during the content calibration calculation of the test sample to ensure the accuracy of the experimental results.

[0059] Table 3 Microwave digestion conditions

[0060] step Climb(min) Maintain (min) Temperature(℃) Power(W) 1 5 5 120 1600 2 5 5 150 1600 3 5 25 180 1600

[0061] 2.3 Content determination method

[0062] The isotopes selected for determination are 208Pb, 75As, 114Cd, and 63Cu, among which 208Pb uses 209Bi as the internal standard, 114Cd uses 115In as the internal standard, and 75As and 63Cu use 72Ge as the internal standard. The online internal standard method is used to pump the test solution and the internal standard solution into the nebulizer using a peristaltic pump and then enter the inductively coupled plasma mass spectrometer, and then perform linear regression according to 2.1 instrument parameters with concentration as the horizontal axis and response value as the vertical axis for determination.

[0063] 2.4 Preparation of standard curve

[0064] Accurately measure appropriate amounts of lead, arsenic, cadmium stock solutions 2 and copper stock solution 1, respectively, and prepare a series of concentration linear relationship investigation solutions according to the standard curve preparation method in "2.2". Determine according to the instrument parameters under "2.1", and perform linear regression with concentration as the horizontal axis and response value as the vertical axis. The linear range and linear equation are detailed in Table 4.

[0065] Table 4 Linear range and linear equation

[0066] Element Name Linear equations R Linear range 208Pb y=3908.1658*x+233.5967 0.9993 0.0ng / ml~20ng / ml 75As y=103.0587*x+1.1100 0.9976 0.0ng / ml~20ng / ml 114Cd y=657.0755*x+3.3367 0.9996 0.0ng / ml~10ng / ml 63Cu y=1214.7182*x+337.0533 1.0000 0.0ng / ml~500ng / ml

[0067] 2.5 Detection line and quantification limit

[0068] Take the test blank and measure it continuously for 11 times according to the instrument parameters in "2.1" to obtain the standard deviation δ of the 11 response values ​​of the test blank. The results are shown in Table 5.

[0069] Table 5 11 response values ​​and standard deviations of the blank samples

[0070] Serial number lead arsenic cadmium copper 1 2536.54 12.44 16.68 584.01 2 2556.48 10.00 16.68 580.67 3 2429.62 13.33 20.02 560.65 4 2423.01 13.33 20.02 580.54 5 2493.04 12.22 16.68 560.59 6 2466.21 12.22 23.36 573.99 7 2519.89 13.33 20.03 577.32 8 2492.91 10.00 20.03 567.24 9 2489.61 12.44 16.68 573.94 10 2523.08 10.00 20.02 587.33 11 2533.10 13.33 22.70 580.67 Standard Deviation δ 43.1939 1.3972 2.4102 8.9954 Standard curve slope 3721.5909 106.317 659.1696 1273.3912

[0071] According to the calculation results in Table 5, the detection limit and quantification limit were calculated according to the following formula:

[0072] The detection limit was calculated according to the formula LOD = 3.3δ / S, where LOD: detection limit; S: slope of the standard curve.

[0073] The limit of quantification was calculated according to the formula LOQ = 10δ / S, where LOQ: limit of quantification: S: slope of the standard curve.

[0074] The detection limit and quantification limit of each element are shown in Table 6.

[0075] Table 6 Detection limits and quantification limits of elements

[0076] name Limit of quantitation (ng / ml) Detection limit (ng / ml) <![CDATA[ 208 Pb]]> 0.1161 0.03830 <![CDATA[ 75 As]]> 0.1314 0.04337 <![CDATA[ 114 Cd]]> 0.03656 0.01207 <![CDATA[ 63 With]]> 0.07064 0.02331

[0077] 2.6 Precision test

[0078] Prepare the reference mixed solutions of lead, arsenic, cadmium and copper with the concentrations of 5 ng / ml, 2 ng / ml, 0.3 ng / ml and 20 ng / ml, inject the samples 6 times continuously according to the instrument parameters under "2.1", calculate the RSD value of each element concentration, and the results are shown in Table 7. The RSD of each element concentration is <15%. The method has good precision and meets the analysis requirements.

[0079] Table 7 Precision test results

[0080]

[0081] 2.7 Determination of recovery rate

[0082] Accurately weigh 9 portions of the test sample, each portion is about 0.1g, and divide them into three groups, each group has three samples. The first group is added with a reference standard solution approximately equivalent to 50% of the test sample limit value, the second group is added with a reference standard solution approximately equivalent to 100% of the test sample limit value, and the third group is added with a reference standard solution approximately equivalent to 150% of the test sample limit value (the spiked concentrations and amounts of the four elements lead, arsenic, cadmium, and copper are detailed in Table 8). The remaining steps are prepared according to the test sample preparation method under "2.2", determined according to the instrument parameters under "2.1", and the recovery test is carried out according to the content determination method under "2.3".

[0083] Table 8 Concentration and amount of spiked elements of lead, arsenic, cadmium and copper

[0084]

[0085]

[0086] The recovery rate was calculated according to the standard curve equation of the reference substance, and the results are shown in Table 9. The recovery rates of each element at different levels were between 75% and 120% for lead, 75% and 120% for arsenic, 70% and 125% for cadmium, and 80% and 115% for copper, and the RSD values ​​were within 6%.

[0087] Table 9 Recovery results

[0088]

[0089]

[0090] 2.8 Sample determination

[0091] Take each batch of test sample, prepare the test sample solution according to "2.2", and measure according to the instrument parameters in "2.1". The results are shown in Table 10.

[0092] Table 10 Sample test results

[0093]

[0094] 2.9 Durability

[0095] Take about 0.1g of the test sample, weigh it accurately, put it in a 50ml digestion tube, add 5ml of nitric acid, leave it overnight, add 1ml of 30% hydrogen peroxide solution before digestion, cover and tighten, put it in a microwave digestion instrument for digestion, microwave digestion conditions are shown in Table 11, after digestion is complete, remove the tube and put it in an acid remover at 80℃ for 30 minutes, take it out and let it cool. Prepare the reagent blank solution in the same way.

[0096] Table 11 Microwave digestion conditions

[0097] step Climb(min) Maintain (min) Temperature(℃) Power(W) 1 5 5 120 1600 2 5 5 150 1600 3 5 25 170 1600

[0098] Carefully transfer the liquid in the digestion tube to a 100 ml volumetric flask, dilute to volume with ultrapure water and shake well. Filter with a microporous filter membrane (0.22 μm), and take the filtrate to obtain the test solution for the determination of lead, arsenic, cadmium and copper elements.

[0099] According to "2.2", 10% nitric acid solution was used to make up the volume, and a series of concentration linear relationship test solutions were prepared. The instrument parameters under "2.1" were measured, and the content determination method under "2.3" was used to perform linear regression with concentration as the horizontal axis and response value as the vertical axis to test the content of the 5 batches of test samples. The results are shown in Table 12.

[0100] Table 12 Durability test results

[0101]

[0102] The RD value results of the average value of the durability content of the five batches of test products and the average value of the sample measured content are shown in Table 13.

[0103] Table 13 RD value results of the average value of durability content and the average value of sample measured content

[0104]

[0105]

[0106] From the data in Table 13, it can be seen that the test results of the two methods are close, and the RD value is less than 8.0%, which means that the test results are not affected by changing conditions and have good durability.

[0107] This application scheme can effectively detect the content of heavy metal elements arsenic (As), cadmium (Cd), copper (Cu) and lead (Pb) in artificial tiger bone powder, which will not only help improve product quality and safety, but also help expand its application scope and promote the development of the traditional Chinese medicine industry; at the same time, these studies will also help to understand the chemical composition and pharmacological action mechanism of Chinese medicinal materials, and provide support for the modernization and internationalization of traditional Chinese medicine.

[0108] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present application, rather than to limit it. Although the present application has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present application.

Claims

1. A method for determining four heavy metal elements in artificial tiger bone powder by inductively coupled plasma mass spectrometry, characterized in that: The following steps are involved: (1) Preparation of solution: Preparation of lead, arsenic and cadmium stock solution 1: put lead single element solution standard substance, arsenic single element solution standard substance and cadmium single element solution standard substance into the same volumetric flask, dilute to scale with solvent, and shake well to obtain lead, arsenic and cadmium stock solution 1; Preparation of lead, arsenic and cadmium stock solution 2: take lead, arsenic and cadmium stock solution 1 and place it in a volumetric flask, dilute to the mark with solvent, and shake well to obtain lead, arsenic and cadmium stock solution 2; Preparation of copper stock solution 1: Place copper single element solution standard substance in a volumetric flask, dilute to scale with solvent, and shake well to obtain copper stock solution 1; Preparation of internal standard solution: Accurately pipette Bi, Ge and In multi-element standard solutions into a volumetric flask, add solvent to make up to the mark, and shake well to obtain a mixed internal standard solution of Bi, Ge and In; (2) Preparation of test solution: accurately weigh the test sample and place it in a digestion tube, add nitric acid, and place it overnight. Before digestion, add hydrogen peroxide solution, cover and tighten, place in a microwave digestion instrument for digestion, remove the digestion tube after digestion is complete, place it in an acid remover to remove acid, remove it and let it cool, transfer the liquid in the digestion tube to a volumetric flask, dilute to the mark with ultrapure water, shake well, filter with a microporous filter membrane, and take the filtrate; (3) Content determination: The online internal standard method is used to pump the test solution and the internal standard solution into the nebulizer using a peristaltic pump and then mix them into the inductively coupled plasma mass spectrometer for determination; (4) Plotting of standard curve: Accurately measure appropriate amounts of lead, arsenic, cadmium stock solution 2 and copper stock solution 1, respectively, to prepare a series of concentration linear relationship test solutions, and perform linear regression with concentration as the horizontal axis and response value as the vertical axis.

2. The method for determining four heavy metal elements in artificial tiger bone powder by inductively coupled plasma mass spectrometry according to claim 1, characterized in that: In step (3), the isotopes selected for determination are 208Pb, 75As, 114Cd and 63Cu, wherein 208Pb uses 209Bi as an internal standard, 114Cd uses 115In as an internal standard, and 75As and 63Cu use 72Ge as an internal standard.

3. The method for determining four heavy metal elements in artificial tiger bone powder by inductively coupled plasma mass spectrometry according to claim 1, characterized in that: In step (2), the usage ratio of the test sample, nitric acid and hydrogen peroxide solution is 0.1 g:8 ml:1 ml.

4. The method for determining four heavy metal elements in artificial tiger bone powder by inductively coupled plasma mass spectrometry according to claim 1, characterized in that: In step (2), the mass fraction of the hydrogen peroxide solution is 30%.

5. The method for determining four heavy metal elements in artificial tiger bone powder by inductively coupled plasma mass spectrometry according to claim 1, characterized in that: In step (2), the acid removal temperature is 80° C. and the acid removal time is 30 minutes.

6. The method for determining four heavy metal elements in artificial tiger bone powder by inductively coupled plasma mass spectrometry according to claim 1, characterized in that: In step (2), the pore size of the filter membrane is 0.22 μm.

7. The method for determining four heavy metal elements in artificial tiger bone powder by inductively coupled plasma mass spectrometry according to claim 1, characterized in that: In step (1), the solvent is a 10% nitric acid solution, and the preparation process of the 10% nitric acid solution is as follows: take 100 ml of nitric acid, add ultrapure water to dilute to 1000 ml, and obtain a 10% nitric acid solution.

8. The method for determining four heavy metal elements in artificial tiger bone powder by inductively coupled plasma mass spectrometry according to claim 1, characterized in that: In step (1), the lead concentration in the lead, arsenic and cadmium stock solution 1 is 10 μg / ml, the arsenic concentration is 10 μg / ml, and the cadmium concentration is 5 μg / ml.

9. The method for determining four heavy metal elements in artificial tiger bone powder by inductively coupled plasma mass spectrometry according to claim 1, characterized in that: In step (1), the lead concentration in the lead, arsenic and cadmium stock solution 2 is 1000ng / ml, the arsenic concentration is 1000ng / ml, and the cadmium concentration is 500ng / ml.

10. The method for determining four heavy metal elements in artificial tiger bone powder by inductively coupled plasma mass spectrometry according to claim 1, characterized in that: In step (1), the concentration of the copper stock solution 1 is 10 μg / ml; or In step (1), the concentration of the mixed internal standard solution of Bi, Ge and In is 500 ng / ml.

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