CN107976481B - Method for detecting scandium content in traditional Chinese medicinal materials - Google Patents
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Abstract
The invention discloses a method for detecting scandium content in traditional Chinese medicinal materials, which adopts an inductively coupled plasma mass spectrometry to analyze, and comprises the following detection steps: (1) preparing a series of standard solutions; (2) preparing an internal standard solution; (3) preparing a sample solution; (4) performing inductively coupled plasma mass spectrometry (ICP-MS) analysis; (5) and calculating to obtain a result. The method disclosed by the invention is simple and convenient to operate, convenient and quick, high in detection efficiency, high in accuracy and precision, and good in stability and reproducibility. The application range of the traditional Chinese medicine heavy metal detection platform is expanded, the quality safety of the traditional Chinese medicine can be better ensured, and technical reserve is provided for measuring the scandium content in the traditional Chinese medicine.
Description
Technical Field
The invention relates to the field of medicine detection, in particular to a method for detecting scandium content in traditional Chinese medicinal materials.
Background
The residues of heavy metals and harmful elements are used as one of exogenous pollutants of the traditional Chinese medicine, and always affect the quality of the traditional Chinese medicine and the impression of the traditional Chinese medicine at home and abroad. Therefore, standards such as ' green industry standards of medicinal plants and preparations ', Chinese pharmacopoeia ' and the like are established in China, and heavy metal residues of the medicinal plants and medicinal materials are controlled so as to guarantee the quality of the medicinal materials. From the existing literature reports and national standards, most researches focus on five elements of lead, arsenic, mercury, cadmium and copper, while detection researches on other elements are relatively few, and corresponding data accumulation is lacked.
Scandium (Sc) is a rare earth element and is present in the earth's crust in very small amounts, only 0.0005%. Because the content of the scandium Sc in the traditional Chinese medicinal materials is extremely low, the scandium Sc is usually used as an internal standard element when the ICP-MS method is adopted to determine the residues of heavy metals and harmful elements, and reports for detecting the content of the scandium Sc in the traditional Chinese medicinal materials are fresh in the existing documents.
The prior publications also relate to the related technology for detecting scandium content, and the following patent documents are searched for the related technology:
1. chinese patent: measuring scandium content in steel; application No.: 01610731169.3, respectively; application date: 2016-08-26; the applicant: inner Mongolia Steel ladle, Union Ltd; and (3) abstract: the invention discloses a method for measuring scandium content in steel, which comprises the following steps: weighing a steel sample, dissolving the steel sample by using mixed acid to prepare a sample test solution, and carrying out a blank test; under the selected working parameters, simultaneously measuring a scandium working curve standard solution and a sample test solution by adopting an inductively coupled plasma mass spectrometer; when measuring the scandium working curve standard solution and the sample test solution, rhodium is used as an internal standard element for measurement, and a blank value is subtracted from a measured value of the sample test solution to obtain an actual value of the steel sample to be measured. The method has the advantages of simple and rapid operation, high sensitivity and high accuracy, and meets the requirements of scientific research and production.
2. Chinese patent: a method for measuring the contents of gallium and scandium in blast furnace smoke dust; application No.: 201310225789.6, respectively; application date: 2013-06-07; the applicant: wu Steel group Kunming Steel works, Inc.; and (3) abstract: the invention provides a method for measuring gallium and scandium content in blast furnace smoke dust, which comprises the steps of measuring the spectral line intensity of a sample solution by using a conventional inductively coupled plasma atomic emission spectrometry, and obtaining corresponding gallium and scandium content values in a standard working curve of gallium and scandium according to the spectral line intensity, and is characterized in that the sample solution is prepared by the following steps: adding sodium hydroxide into the sample to melt the sample at high temperature, leaching the melted sample with hot water to obtain a solution, dissolving sodium hydroxide precipitate in the solution with hydrochloric acid, and acidifying the test solution with hydrochloric acid to obtain a sample solution to be tested. After the method provided by the invention dissolves the sample, the contents of gallium and scandium in the blast furnace smoke dust can be directly measured, the operation is convenient, the accuracy of the measured contents of gallium and scandium is high, the measured result has good stability, reproducibility and accuracy, and the requirement of daily measurement of the contents of gallium and scandium in the blast furnace smoke dust can be completely met.
Disclosure of Invention
The invention aims to expand the application range of a detection platform for heavy metals and harmful elements in traditional Chinese medicinal materials and ensure the quality safety of the traditional Chinese medicinal materials, and provides a detection method for scandium content in the traditional Chinese medicinal materials.
The invention is realized by the following technical scheme:
a method for detecting scandium content in traditional Chinese medicinal materials comprises the following steps:
(1) preparation of a series of standard solutions: scandium single element standard solution (1000 mg. L) is precisely absorbed-1) Diluting with 2% nitric acid solution to obtain scandium with concentration of 0.1 μ g/L-1、0.5μg·L-1、1μg·L-1、5μg·L-1、10μg·L-1The series of standard solutions of (1).
(2) Preparation of internal standard solution: precisely absorbing a proper amount of germanium standard solution, placing the germanium standard solution into a measuring flask, adding 5% nitric acid solution to prepare the germanium standard solution with the concentration of 500 mu g.L-1The internal standard solution of (4).
(3) Preparation of sample solution: taking 0.4-0.8 g of a sample which is crushed into coarse powder, precisely weighing, placing the sample in a digestion tank, and adding the mixture into a digestion tank according to the volume ratio of 7-8: 0.5-1 of nitric acid-hydrofluoric acid mixed acid, uniformly mixing, and then placing in a microwave digestion instrument for digestion according to a certain program; and (3) after digestion, cooling, placing on an acid-dispelling frame for dispelling acid at 125-135 ℃ for dispelling acid for 2-3 hours, cooling to room temperature, transferring into a 25ml volumetric flask, washing the digestion tank with a nitric acid solution with the volume concentration of 2% for 3-5 times, and diluting to a scale to obtain a sample solution.
(4) Inductively coupled plasma mass spectrometry (ICP-MS) analysis was performed: respectively and precisely absorbing a series of standard solutions and sample solutions, injecting the solutions into an inductively coupled plasma mass spectrometer, and analyzing and determining according to certain conditions.
(5) And calculating to obtain a result: scandium content was determined from the standard curve.
The microwave digestion program is as follows: the temperature is programmed to rise with the power of 1030-1800W, the climbing time is 20-25 min, and the temperature is kept at 190 ℃ for 20-25 min.
The operating parameters of the inductively coupled plasma mass spectrometry (ICP-MS) analysis are as follows: radio frequency power 1550W; the sampling depth is 10 mm; carrier gas flow rate 1.09 L.min-1(ii) a He collision mode is adopted, and the flow rate of He gas is 3.4 mL/min-1(ii) a Integration time 2S; the scan type is single bar. The isotope selected in the measurement is45Sc of at least one of72Ge is an internal standard.
The detection conditions and the method adopted by the invention are screened after a plurality of times of experimental exploration and research on the basis of looking up a large amount of documents, and can achieve the purposes of high accuracy, high precision, low detection limit, good stability and the like.
The invention has the beneficial effects that:
1. the method for detecting the scandium content in the traditional Chinese medicinal materials expands the application range of a traditional Chinese medicinal material heavy metal detection platform, can better ensure the quality safety of the traditional Chinese medicinal materials, and provides technical reserve for measuring the scandium content in the traditional Chinese medicinal materials.
2. The method for detecting the content of scandium in the traditional Chinese medicinal materials adopts inductively coupled plasma mass spectrometry (ICP-MS) for analysis, is simple and convenient to operate, convenient and rapid, and has high detection efficiency, high accuracy, high precision and good stability and reproducibility.
Detailed Description
In order to describe the present invention in more detail, the present invention will be further described with reference to the following examples. The embodiments are not intended to limit the technical solutions of the present invention, and all modifications made within the scope of the claims of the present invention are still within the scope of the claims of the present invention.
The instruments and reagents used were: agilent 8800 inductively coupled plasma mass spectrometer; millipore Mill-Q ultra pure water machine; CEM MARS6 microwave digestion instrument; model ML204 electronic analytical balance (mettler-toledo instruments ltd). Standard scandium Single element solution available from Shanghai spectral company, manufacturer O2Si, specification 1000 mg.L-1Batch number 1064277. The standard substances such as citrus leaves, spirulina, pollen and the like are purchased from the institute of geophysical and geochemical investigation of Chinese geological academy. The standard solution of germanium single element is purchased from Jinan Zhonggao science and technology Limited and has a specification of 1000 mug· -1mLLot number ZBR 321; containing Ce, Co, Li6Tuning solutions of Mg, Tl, Y (1. mu. u.)g· -1L) From Agilent, inc. Nitric acid is high grade pure MERCK, hydrofluoric acid is high grade pure, hydrogen peroxide is high grade pure, and water is high purity water treated by a water purifier.
Example 1
A method for detecting scandium content in traditional Chinese medicinal materials comprises the following steps:
(1) preparation of a series of standard solutions: scandium single element standard solution (1000 mg. L) is precisely absorbed-1) 1mL, placing the solution into a 100mL measuring flask, adding a 2% nitric acid solution to dilute the solution to a scale mark to obtain a scandium standard solution (10 mg. L)-1) Precisely sucking 0.25mL of the standard solution, placing in a 10mL measuring flask, adding 2% nitric acid solution, and diluting to scale to obtain scandium stock solution (0.25 mg. L)-1). Accurately sucking scandium stock solution 0.01mL, 0.05 mL, 0.1 mL, 0.5mL, 1mL, placing into 25mL measuring flask, adding 2% nitric acid solution, diluting to scale to obtain scandium concentration of 0.1 μ g.L-1、0.5μg·L-1、1μg·L-1、5μg·L-1、10μg·L-1The series of standard solutions of (1).
(2) Preparation of internal standard solution: precisely absorbing a proper amount of germanium standard solution, placing the germanium standard solution into a measuring flask, adding 5% nitric acid solution to prepare the germanium standard solution with the concentration of 500 mu g.L-1The internal standard solution of (4).
(3) Preparation of sample solution: taking 0.5g of a sample which is crushed into coarse powder, precisely weighing, placing the coarse powder in a digestion tank, adding 8mL of nitric acid and 0.5mL of hydrofluoric acid, uniformly mixing, and then placing the mixture in a microwave digestion instrument for digestion according to a certain program; and (3) after digestion, cooling, placing on an acid-dispelling frame for dispelling acid at 130 ℃ for 2.5 hours, cooling to room temperature, transferring into a 25ml volumetric flask, washing the digestion tank with a nitric acid solution with the volume concentration of 2% for 3-5 times, and diluting to a scale to obtain a sample solution.
(4) Inductively coupled plasma mass spectrometry (ICP-MS) analysis was performed: respectively and precisely absorbing a series of standard solutions and sample solutions, injecting the solutions into an inductively coupled plasma mass spectrometer, and analyzing and determining according to certain conditions.
(5) And calculating to obtain a result: scandium content was determined from the standard curve.
The microwave digestion program is as follows: the temperature is programmed to rise, the power is 1030-1800W, the climbing time is 20-25 min, and the temperature is kept at 190 ℃ for 20 min.
The operating parameters of the inductively coupled plasma mass spectrometry (ICP-MS) analysis are as follows: radio frequency power 1550W; the sampling depth is 10 mm; carrier gas flow rate 1.09 L.min-1(ii) a He collision mode is adopted, and the flow rate of He gas is 3.4 mL/min-1(ii) a IntegrationTime 2S; the scan type is single bar. The isotope selected in the measurement is45Sc of at least one of72Ge is an internal standard.
The methodology of the test described in the examples was tested for validation as follows:
1. investigation of kinds and amounts of digestion solvents
Three quality control substances with an uncertain range, namely citrus leaves, spirulina and pollen are adopted to investigate the digestive solvent. Taking 0.5g of each quality control substance powder, precisely weighing, placing in a digestion tank, adding different digestion solvents, placing in a microwave digestion instrument for digestion, adopting an Onedouch mode for temperature program rise, and climbing time: and (3) 20-25 min, raising the temperature to 190 ℃, keeping the temperature for 20min, keeping the power at 1030-1800W, cooling after the temperature is up, transferring the cooled liquid into a 25mL measuring flask with water, diluting the liquid to a scale, shaking up the liquid, and performing sample injection and measurement. As a result, the measured value of the citrus leaves is within the specified range but close to the bottom limit of the specified value by using only nitric acid for digestion; when the digestion system of nitric acid plus hydrofluoric acid was used, the measured values of the three standard substances were close to the median of the predetermined interval, and thus the digestion solvent was determined to be 8mL of nitric acid plus 0.5mL of hydrofluoric acid, as shown in Table 1.
TABLE 1 investigation results of different digestion solvents
2. Influence of acid removal
According to the preparation method of the sample solution, the influence of acid-dispelling for 2.5h at 130 ℃ after nitric acid digestion and the influence of acid-dispelling failure on scandium determination results are respectively compared. The results show that: acid was removed with little effect on the assay results, see table 2. In order to reduce the corrosion of hydrofluoric acid to the instrument, the acid is removed for 2.5h at 130 ℃ after the sample is digested.
TABLE 2 Deacidification effects investigation results
3. Investigation of linear relationships
Sampling a series of standard solutions to obtain a regression equation: y =0.0814X +0.0027, R =1.0000, indicating good linearity when the injection concentration is 0.1ng/ml to 10 ng/ml.
4. Repeatability survey
Taking six parts of citrus leaves, each part of which is 0.5g, precisely weighing, placing the six parts in a digestion tank, adding 8mL of nitric acid solution and 0.5mL of hydrofluoric acid, uniformly mixing, placing the mixture in a microwave digestion instrument for digestion, cooling, placing the mixture on an acid rack for acid removal for 2.5 hours at 130 ℃, cooling, transferring the mixture into a 25mL measuring flask by using 2% nitric acid solution, diluting to scale, shaking uniformly, and carrying out sample injection measurement. The RSD of the six samples was 4.40% and the reproducibility met the methodology requirements, the results are shown in table 3.
TABLE 3 results of repeated investigation
5. Precision survey
Sample solution under the repeatability item is taken and continuously injected for 6 times, the RSD of the measured concentration is 0.45 percent, the methodological requirement is met, and the result is shown in table 4.
TABLE 4 results of precision examination
6. Stability survey
Sample solution under the repeatability item is taken, sample injection is carried out at intervals within 24 hours for determination, the RSD of the determination concentration is 4.25%, the sample is stable within 24 hours, and the result is shown in Table 5.
Table 5 stability test results
7. Sample application recovery test
Taking six parts of citrus leaf, each 0.5g, precisely weighing, placing in a digestion tank, and precisely adding scandium stock solution (0.25 mg. L)-1) 0.3mL, preparing sample adding solution according to the repeatability, carrying out sample injection measurement, calculating sample adding recovery rate, wherein the result recovery rate is between 90 and 120 percent, and the trace analysis is satisfiedAnd (6) obtaining.
TABLE 6 sample recovery test results
A methodology investigation result shows that the method can be used for detecting the content of scandium in the traditional Chinese medicinal material.
Claims (2)
1. A method for detecting scandium content in traditional Chinese medicinal materials is characterized by comprising the following steps:
(1) preparation of a series of standard solutions: the precise absorption concentration is 1000 mg.L-1The scandium single element standard solution is diluted by adding 2 percent nitric acid solution to prepare scandium with the concentration of 0.1 mu g.L respectively-1、0.5μg·L-1、1μg·L-1、5μg·L-1、10μg·L-1A series of standard solutions of (a);
(2) preparation of internal standard solution: precisely absorbing a proper amount of germanium standard solution, placing the germanium standard solution into a measuring flask, adding 5% nitric acid solution to prepare the germanium standard solution with the concentration of 500 mu g.L-1The internal standard solution of (4);
(3) preparation of sample solution: taking 0.4-0.8 g of a sample which is crushed into coarse powder, precisely weighing, placing the sample in a digestion tank, and adding the mixture into a digestion tank according to the volume ratio of 7-8: 0.5-1 of nitric acid-hydrofluoric acid mixed acid, uniformly mixing, and then placing in a microwave digestion instrument for digestion according to a certain program; after digestion, cooling, placing on an acid-dispelling frame for dispelling acid at 125-135 ℃ for 2-3 hours, cooling to room temperature, transferring into a 25ml volumetric flask, washing the digestion tank with a nitric acid solution with the volume concentration of 2% for 3-5 times, and diluting to a scale to obtain a sample solution;
(4) performing inductively coupled plasma mass spectrometry: respectively and precisely absorbing a series of standard solutions and sample solutions, injecting the solutions into an inductively coupled plasma mass spectrometer, and analyzing and determining according to certain conditions;
the working parameters of the inductively coupled plasma mass spectrometry are as follows: radio frequency power 1550W; the sampling depth is 10 mm; carrier gas flow rate 1.09 L.min-1(ii) a He collision mode is adopted, and the flow rate of He gas is 3.4 mL/min-1(ii) a Integration time 2S; the scanning type is a single-rod type,the isotope selected in the measurement is45Sc of at least one of72Ge is an internal standard;
(5) and calculating to obtain a result: scandium content was determined from the standard curve.
2. The method for detecting the scandium content in the traditional Chinese medicinal material as claimed in claim 1, wherein the microwave digestion program is as follows: the temperature is programmed to rise with the power of 1030-1800W, the climbing time is 20-25 min, and the temperature is kept at 190 ℃ for 20-25 min.
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