CN114414556B - Detection method for measuring 12 elements in astragalus membranaceus by dry ashing-lithium metaborate alkali fusion - Google Patents
Detection method for measuring 12 elements in astragalus membranaceus by dry ashing-lithium metaborate alkali fusion Download PDFInfo
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
Abstract
The invention discloses a detection method for measuring 12 elements in astragalus membranaceus by dry ashing-lithium metaborate alkali fusion, which comprises the steps of gradually ashing a traditional Chinese medicine astragalus membranaceus sample in a muffle furnace, adding lithium metaborate alkali fusion, carrying out ultrasonic leaching by dilute HCl solution, carrying out constant volume shaking, carrying out inductively coupled plasma emission spectrometry (ICP-OES) test, analyzing spectral line intensity response values of all elements, and quantifying all elements of the sample through a standard curve. The method establishes a method for measuring 12 elements such as silicon aluminum in astragalus by step ashing-lithium metaborate alkali fusion-inductively coupled plasma emission spectrometry (ICP-OES), the test quality technical indexes can meet the analysis requirement of actual samples, the precision of each element is within 10%, the requirements of the analysis method in general rule 9101 of the pharmacopoeia of the people's republic of China are met, and scientific basis is provided for the safe production of astragalus.
Description
Technical Field
The invention relates to the technical field of determination of 12 elements in astragalus, in particular to a detection method for determining 12 elements in astragalus by dry ashing-lithium metaborate alkali fusion.
Background
The Chinese medicinal materials are raw materials of the Chinese medicinal decoction pieces and the formulated preparation, and the quality of the Chinese medicinal materials is directly related to clinical medication safety and curative effect, so the quality control of the Chinese medicinal materials is particularly important. Meanwhile, along with the worldwide application of traditional Chinese medicinal materials, the quality control of the traditional Chinese medicinal materials ensures the safety, stability, effectiveness and controllability of the traditional Chinese medicines, and realizes the core problems of modernization, industrialization and internationalization of the traditional Chinese medicines. The quality of the Chinese medicinal materials from different producing areas is comprehensively influenced by factors such as seed sources, producing area climate, soil, harvesting period, medicament application position, processing method and the like. In order to ensure the safety, effectiveness, stability and controllability of the medicine, screen good varieties and promote reasonable development and utilization of resources, the quality evaluation of the traditional Chinese medicine becomes a hotspot and a focus in the current research. Because the curative effect of the traditional Chinese medicine is the result of the synergistic effect of a plurality of components, the curative effect of the traditional Chinese medicine is closely related to the types and the contents of organic components and inorganic elements. Each Chinese medicinal material contains a plurality of inorganic elements, the elements are mutually connected, and research on the inorganic elements in the Chinese medicinal materials is one of ways for uncovering the mechanism of the Chinese medicinal properties.
Astragalus root is one of the commonly used clinical traditional Chinese medicines, has sweet taste and slight warmth, enters spleen and lung channels, and can tonify middle-jiao and qi, strengthen superficies and induce diuresis, promote pus discharge and promote granulation. As a result of recent researches on astragalus mongholicus by combing a plurality of scholars, the main chemical components of astragalus mongholicus comprise polysaccharides, saponins, flavonoids, amino acids, inorganic elements, sterols and the like; pharmacological actions of astragalus include anti-tumor, protecting cardiac and cerebral vessels, improving immune function, protecting lung function, protecting kidney tissue, protecting liver injury, protecting intestinal function, regulating blood pressure, resisting aging, preventing and treating osteoporosis, protecting against oxidative stress, protecting peritoneum, protecting against radiation, protecting retinal ganglion cells, insulin sensitization, preventing and treating diabetic vascular complications, etc. Along with the gradual deep research on the physiological and pharmacological activities of traditional Chinese medicines in recent years and the rapid development of the inorganic chemistry field, research reports at home and abroad show that inorganic elements are one of the effective components of traditional Chinese medicines in traditional Chinese medicines such as astragalus mongholicus and the like, and have extremely important significance on clinical treatment effects.
Si contained in the Chinese medicinal materials can promote metabolism of human skeleton, strengthen skeleton, prevent and treat cardiovascular and cerebrovascular diseases, reduce blood pressure and resist aging, and free SiO 2 Is the main substance for causing silicosis; al compounds can cause dermatitis, bronchial asthma and other diseases, al accumulated in human tissues can cause senile dementia, and high-concentration Al in the environment is also a toxic factor causing death of fishes and a large amount of water organisms; researches show that the traditional Chinese medicine with the effects of calming liver wind, clearing heat, promoting blood circulation, tonifying kidney and strengthening yang has higher Zn content; cu, fe, mn and the like have important influences on physiological functions of a human body. Therefore, accurate determination of Si, al and other elements in the traditional Chinese medicine materials is quite important.
Currently, methods for elemental analysis in geologic samples and foods are mainly inductively coupled plasma emission spectrometry (ICP-OES), inductively coupled plasma mass spectrometry (ICP-MS), atomic Absorption Spectrometry (AAS). The detection of the traditional Chinese medicinal materials mainly refers to the general rule 9304, general rule 0411 and 0412 of the pharmacopoeia of the people's republic of China, and the microwave digestion, pressure tank digestion, wet digestion and dry digestion in the method are not applicable to Si and Al, and the dissolution is incomplete, so that the result value is lower; the direct alkali fusion is easy to cause high blank value, the salt content of the solution is high, the detection limit is affected, and because a large amount of Na salt is introduced and Na and Mg in the solution to be detected cannot be measured simultaneously, the pretreatment problem of simultaneously measuring Si, al and other elements of the traditional Chinese medicine sample is difficult to solve.
Disclosure of Invention
At present, no standard method for measuring Si, al and the like in Chinese herbal medicines is established in China. The method firstly provides an analysis method for measuring Si, al, K, ca, na, mg, fe, P, S, zn, ti in astragalus membranaceus by adopting a gradual ashing-lithium metaborate alkali fusion-inductively coupled plasma emission spectrometry (ICP-OES), and realizes the simultaneous analysis of Si, al, S, P, zn and other elements.
The purpose of the invention is as follows:
(1) The method provides a feasible method for analyzing Si, al, S and other elements in the astragalus Chinese medicinal materials, can be used for referencing other Chinese medicinal materials, and can rapidly and accurately analyze the distribution and content characteristics of each element in the Chinese medicinal materials.
(2) Has important academic value in pharmacological research, clinical application and other aspects of astragalus.
(3) Provides technical basis for quality control and effective evaluation of traditional Chinese medicinal materials such as astragalus membranaceus and the like.
(4) The establishment of the method can ensure the safety, effectiveness, stability and controllability of the astragalus Chinese medicinal materials, and provides technical support for screening good varieties and promoting reasonable development and utilization of resources.
In order to achieve the aim, the invention provides a detection method for measuring 12 elements in astragalus membranaceus by dry ashing-lithium metaborate alkali fusion.
In order to achieve the above purpose, the present invention provides the following technical solutions:
and gradually ashing a traditional Chinese medicine astragalus sample in a muffle furnace, adding lithium metaborate, carrying out ultrasonic leaching by using a dilute HCl solution, uniformly shaking to a constant volume, carrying out inductively coupled plasma emission spectrometry (ICP-OES) test, analyzing the response value of the spectral line intensity of each element, and quantifying each element of the sample through a standard curve.
The method comprises the following steps:
a detection method for measuring 12 elements in astragalus root by dry ashing-lithium metaborate alkali fusion comprises the following steps:
s1, sample pretreatment
Cleaning radix astragali, slicing, and drying (oven drying, air drying, drying in shade, etc.), wherein the drying temperature should be controlled below 60deg.C. And (3) carrying out manual or mechanical grinding on the initially prepared sample by adopting an agate mortar, and enabling the sample to completely pass through a nylon sieve with the sieve aperture of 0.25-0.4mm, and uniformly mixing. The mixture was divided into the desired amounts by the quartering method. The uniformly mixed sample is paved into a circle, the cross line drawn by the cross line is divided into four equal parts, two diagonal parts are taken, and the mixture is continuously divided into required amounts.
S2, weighing the sample in a platinum crucible, and ashing in a muffle furnace
Weighing 0.2500g of astragalus sample powder in a platinum crucible, ashing in a muffle furnace, half-masking a furnace door, heating to 140 ℃, and keeping the temperature at 140 ℃ to 400 ℃ for 20min every 20 ℃ after heating; maintaining at 400-600 deg.C for 30min at 50 deg.C; taking out and cooling;
s3, adding lithium metaborate for melting and dilute HCl for ultrasonic leaching
Adding 0.1g of lithium metaborate into ash, uniformly stirring, putting into a muffle furnace, melting at 950 ℃ for 15min, taking out, cooling, adding 20mL of 10% diluted hydrochloric acid, placing a platinum crucible into an ultrasonic cleaning instrument, performing ultrasonic leaching until molten crystals are completely dissolved, transferring and fixing the volume to a 50mL plastic volumetric flask, and shaking uniformly to be measured;
s4, measuring by adopting an inductively coupled plasma emission spectrometry
a. On-machine test
According to the working conditions of the instrument in Table 2, an inductively coupled plasma emission spectrometry is adopted for analysis and testing; the same method is used for making a reagent blank test;
the operating conditions of ICP-OES are shown in Table 2;
TABLE 2 list of operating conditions for ICP-OES
b. Drawing of a Standard Curve
Analyzing the mixed standard working solution of each element according to the instrument condition of the a, drawing a standard working curve by taking the concentration as an abscissa and the analysis spectral line intensity response value as an ordinate, and quantifying the sample by using the standard working curve to ensure that the response value of each element is in a measurement linear range; the standard series mass concentration of each element is shown in Table 3;
TABLE 3 standard solution series Mass concentration of elements in ICP-OES method
c. Recommended wavelength of use
The recommended use element wavelengths are shown in table 4;
TABLE 4 test elements and analytical spectral lines
S5, method establishment-result calculation
The content of each element in the astragalus is calculated according to the following formula:
wherein:
x is the content of the element to be detected in the astragalus sample, and the unit is mg/L;
rho-mass concentration of the element to be detected in the astragalus sample solution, the unit is mg/L;
ρ 0 the mass concentration of the element to be detected in the blank liquid is mg/L;
v-the constant volume of the digestive juice of the astragalus sample is in mL;
f-dilution of radix astragali sample;
m-weighing the mass of the astragalus sample, wherein the unit is g;
the result of the calculation retains three significant digits.
The method for analyzing Si, al, na, mg, K, ca, P, S, zn, ti, mn, fe in astragalus Chinese herbal medicine by adopting dry ashing-lithium metaborate alkali fusion-inductively coupled plasma emission spectrometry (ICP-OES) is provided for the first time, and the method has the following advantages according to technical characteristics and analysis summary of actual application conditions:
(1) The method combines the current testing situation of elements such as Si, al and the like, establishes a method for measuring 12 elements such as silicon aluminum and the like in the astragalus by step ashing-lithium metaborate alkali fusion-inductance coupling plasma emission spectrometry (ICP-OES) through comparing and analyzing the conditions such as the addition amount of flux, digestion conditions, digestion time, digestion reagent, element analysis spectral line and the like in the astragalus inorganic element detection, ensures that the testing quality technical indexes can meet the analysis requirement of actual samples, ensures that the precision of each element is within 10 percent, meets the requirement of an analysis method in the general rule 9101 of the pharmacopoeia of the people's republic of China, and provides scientific basis for the safe production of the astragalus.
(2) The reagent blank is low, the precision and the accuracy are good, and the reagent can be used for mass detection work.
(3) The quantitative analysis of Si, al, na, mg, K, ca, P, S, zn, ti, mn, fe in the astragalus Chinese medicinal material is realized, the detection limit of each element method (see table 1) is reached, and the precision (RSD) is within 10%. And (3) determining the standard substance astragalus membranaceus, wherein RE values of all elements are-4.06% -7.29%, and the analysis requirements of actual samples are met.
(4) Provides a feasible method for simultaneous analysis of Si, al, na, mg, K, ca, P, S, zn, ti, mn, fe in Chinese medicinal materials such as astragalus and the like, and fills the technical blank of Si, al, na, mg, K, ca, P, S, zn, ti, mn, fe detection in the Chinese medicinal materials.
Table 1 method detection limit
Drawings
FIG. 1 is a flow chart of the whole method of the invention.
FIG. 2 is a flow chart of detection and analysis of 12 elements in astragalus root by dry ashing-lithium metaborate alkali fusion.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
A detection method for measuring 12 elements in astragalus root by dry ashing-lithium metaborate alkali fusion comprises the following steps: 1. sample pretreatment
Cleaning radix astragali, slicing, and drying (oven drying, air drying, drying in shade, etc.), wherein the drying temperature should be controlled below 60deg.C. And (3) carrying out manual or mechanical grinding on the initially prepared sample by adopting an agate mortar, and enabling the sample to completely pass through a nylon sieve with the sieve aperture of 0.25-0.4mm, and uniformly mixing. The mixture was divided into the desired amounts by the quartering method. The uniformly mixed sample is paved into a circle, the cross line drawn by the cross line is divided into four equal parts, two diagonal parts are taken, and the mixture is continuously divided into required amounts.
2. Main instrument and equipment
2.1 inductively coupled plasma emission spectrometer (ICP-OES) (725 model, agilent Inc., U.S.A.).
2.2 ultrasonic cleaning instrument (2300 TH type, shanghai An Spectrum laboratory technologies Co., ltd.).
2.3 balance: the amount was 0.1mg.
2.4 muffle furnace.
2.5 platinum crucible.
3. Reagents and materials
The reagent used in the method meets the experimental requirements, and the water is primary water specified by GB/T6682
3.1 standard solution:
si, al (national non-ferrous metals and electronic materials analysis test center): 10mg/mL;
na, mg, K, ca, fe, P Unit element standard stock solution (national academy of sciences of metering): 1000 μg/mL;
standard stock solution of S-elemental (national non-ferrous metals and electronic materials analysis test center):
1000 μg/mL; zn, ti, mn mixed standard stock solution (national nonferrous metals and electronic materials analysis test center): 100. Mu.g/mL.
3.2 hydrochloric acid (HCl): high-grade purity.
3.3 lithium metaborate (LiBO) 2 ): analytically pure.
3.4 argon (Ar): argon (99.995%) or liquid argon.
4. Analytical procedure
4.1 Low temperature ashing
Weighing 0.2500g of astragalus sample powder in a platinum crucible, ashing in a muffle furnace, half-masking a furnace door, heating to 140 ℃, and keeping the temperature at 140 ℃ to 400 ℃ for 20min every 20 ℃ after heating; maintaining at 400-600 deg.C for 30min at 50 deg.C; taking out and cooling.
4.2 melting of lithium metaborate
Adding 0.1g of lithium metaborate into ash, stirring uniformly, putting into a muffle furnace, melting for 15min at 950 ℃, taking out, cooling, adding 20mL of 10% diluted hydrochloric acid, placing a platinum crucible into an ultrasonic cleaning instrument, performing ultrasonic leaching until molten crystals are completely dissolved, transferring and fixing the volume to a 50mL plastic volumetric flask, and shaking uniformly to be measured.
4.3 on-machine testing
Analytical tests were performed according to the instrument operating conditions of table 2. Reagent blank test was performed in the same manner.
The operating conditions of ICP-OES are shown in Table 2.
4.4 drawing of a Standard Curve
And (3) analyzing the mixed standard working solution of each element according to the instrument condition of 4.3, drawing a standard working curve by taking the concentration as an abscissa and the analysis spectral line intensity response value as an ordinate, and quantifying the sample by using the standard working curve to ensure that the response value of each element is in a measurement linear range. The standard series mass concentrations of each element are shown in Table 3.
4.5 recommended wavelength of use
The wavelengths of the recommended elements are shown in Table 4.
5. Result calculation
The content of each element in the astragalus is calculated according to the following formula:
wherein:
x is the content of the element to be detected in the astragalus sample, and the unit is mg/L;
rho-mass concentration of the element to be detected in the astragalus sample solution, the unit is mg/L;
ρ 0 the mass concentration of the element to be detected in the blank liquid is mg/L;
v-the constant volume of the digestive juice of the astragalus sample is in mL;
f-dilution of radix astragali sample;
m-weighing the mass of the astragalus sample, wherein the unit is g;
the result of the calculation retains three significant digits.
6. Precision of
6.1 repeatability requirements
The ratio (percentage) of the absolute difference of the two independent measurements obtained under repetitive conditions to their arithmetic mean should be 15% or less.
6.2 instrument stability check
When continuous sample injection analysis is carried out, every 20 samples are analyzed, a calibration curve middle concentration point is analyzed, and the relative deviation of analysis and test of detection items is controlled within 10%.
7. Quality assurance and control
7.1 blank test: at least two blank samples are analyzed in each batch, and the test result of the blank samples is lower than the detection limit of the method.
7.2 calibration
The standard curve at least comprises 5 non-zero concentration points, the concentration range of the measured sample is covered, and the correlation coefficient r of the calibration curve is more than or equal to 0.999.
7.3 parallel assay
A parallel should be analyzed for every 20 samples or every batch (less than 20 samples/batch) and the relative deviation of the parallel sample measurements should be less than or equal to 10%.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and principles of the invention are intended to be included within the scope of the invention.
Claims (4)
1. The method for detecting 12 elements in astragalus root by dry ashing-lithium metaborate alkali fusion is characterized by comprising the following steps:
s1, sample pretreatment
Cleaning radix astragali, slicing, and drying at 60deg.C; carrying out manual or mechanical grinding on the preliminarily prepared sample by adopting an agate mortar, and enabling the sample to completely pass through a nylon sieve with the sieve aperture of 0.25-0.4mm, and uniformly mixing; dividing the mixture into required amounts by a quartering method; spreading the uniformly mixed sample into a circle, dividing the cross line drawn by the central line into four equal parts, taking two parts of diagonal lines, and continuing dividing until the required amount is reached;
s2, weighing the sample in a platinum crucible, and ashing in a muffle furnace
Weighing 0.2500g of astragalus sample powder in a platinum crucible, ashing in a muffle furnace, half-masking a furnace door, heating to 140 ℃, and keeping the temperature at 140 ℃ to 400 ℃ for 20min every 20 ℃ after heating; maintaining at 400-600 deg.C for 30min at 50 deg.C; taking out and cooling;
s3, adding lithium metaborate for melting and dilute HCl for ultrasonic leaching
Adding 0.1g of lithium metaborate into ash, uniformly stirring, putting into a muffle furnace, melting at 950 ℃ for 15min, taking out, cooling, adding 20mL of 10% diluted hydrochloric acid, placing a platinum crucible into an ultrasonic cleaning instrument, performing ultrasonic leaching until molten crystals are completely dissolved, transferring and fixing the volume to a 50mL plastic volumetric flask, and shaking uniformly to be measured;
s4, measuring by adopting an inductively coupled plasma emission spectrometry
a. On-machine test
According to the working conditions of the instrument in Table 2, an inductively coupled plasma emission spectrometry is adopted for analysis and testing; the same method is used for making a reagent blank test;
the operating conditions of ICP-OES are shown in Table 2;
TABLE 2 list of operating conditions for ICP-OES
b. Drawing of a Standard Curve
Analyzing the mixed standard working solution of each element according to the instrument condition of the a, drawing a standard working curve by taking the concentration as an abscissa and the analysis spectral line intensity response value as an ordinate, and quantifying the sample by using the standard working curve to ensure that the response value of each element is in a measurement linear range; the standard series mass concentration of each element is shown in Table 3;
TABLE 3 standard solution series Mass concentration of elements in ICP-OES method
c. Recommended wavelength of use
The recommended use element wavelengths are shown in table 4;
TABLE 4 test elements and analytical spectral lines
S5, method establishment-result calculation
The content of each element in the astragalus is calculated according to the following formula:
wherein:
x is the content of the element to be detected in the astragalus sample, and the unit is mg/L;
rho-mass concentration of the element to be detected in the astragalus sample solution, the unit is mg/L;
ρ 0 the mass concentration of the element to be detected in the blank liquid is mg/L;
v-the constant volume of the digestive juice of the astragalus sample is in mL;
f-dilution of radix astragali sample;
m-weighing the mass of the astragalus sample, wherein the unit is g;
the result of the calculation retains three significant digits.
2. The method for detecting 12 elements in astragalus membranaceus by dry ashing-lithium metaborate alkali fusion according to claim 1, which is characterized by comprising the following steps: in the step S1, the drying method is as follows: drying, airing and drying in the shade.
3. The method for detecting 12 elements in astragalus membranaceus by dry ashing-lithium metaborate alkali fusion according to claim 1, which is characterized by comprising the following steps: further comprises:
a. repeatability requirements
The ratio (percentage) of the absolute difference of the two independent measurement results obtained under the repeatability condition to the arithmetic average value thereof is less than or equal to 15%;
b. instrument stability inspection
When continuous sample injection analysis is carried out, every 20 samples are analyzed, a calibration curve middle concentration point is analyzed, and the relative deviation of analysis and test of detection items is controlled within 10%.
4. The method for detecting 12 elements in astragalus membranaceus by dry ashing-lithium metaborate alkali fusion according to claim 1, further comprising the steps of:
a. blank test: at least two blank samples are analyzed in each batch, and the test result of the blank samples is lower than the detection limit of the method;
b. calibration of
The standard curve at least comprises 5 non-zero concentration points, the concentration range of a measured sample is covered, and the correlation coefficient r of the standard curve is more than or equal to 0.999;
c. parallel measurement
A parallel should be analyzed for every 20 samples or every batch (less than 20 samples/batch) and the relative deviation of the parallel sample measurements should be less than or equal to 10%.
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