CN110658276A - Folium artemisiae argyi quality assessment method - Google Patents
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Abstract
The invention provides quality assessment of folium artemisiae argyi, which comprises the following steps: s1 weighing 0.8-1.2g of folium artemisiae argyi powder into a headspace bottle, adding 7-12ml of water, sealing the headspace bottle, shaking uniformly, standing for 20-40min to obtain a test solution, preparing a reference solution, measuring the reference solution and 1ml of headspace gas in the test solution, injecting the reference solution and 1ml of headspace gas into a gas chromatography-mass spectrometer, and analyzing the obtained chromatogram-mass spectrogram to obtain the content of each main component in the folium artemisiae argyi; s2, weighing 0.15-0.35g of folium artemisiae argyi powder into a digestion tank, adding 8-10ml of nitric acid, standing overnight, digesting, dispelling acid, fixing the volume, shaking up, filtering to obtain an upper computer sample solution, and testing the upper computer sample solution by using an inductively coupled plasma mass spectrometer to obtain the content of inorganic elements; s3, according to the contents of the main components and the inorganic elements in the folium artemisiae argyi, the quality of the folium artemisiae argyi is evaluated, and further the quality evaluation result of the folium artemisiae argyi can be comprehensively and accurately obtained.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicine preparations, in particular to a quality evaluation method of folium artemisiae argyi.
Background
Folium artemisiae argyi is a dry leaf of Artemisia argyi (Levl. et Vant) belonging to the family Compositae, has the effects of warming meridians to stop bleeding, dispelling cold to stop pain, eliminating dampness to relieve itching, is a recognized and used plant, and is recorded in Shijing and Huangdi's Nei Jing. In recent years, with the extensive development of folium artemisiae argyi research, the research finds that the pharmacodynamic basis of the folium artemisiae argyi is derived from a large amount of volatile components, flavonoid, tannin, polysaccharide and other complex chemical components contained in the folium artemisiae argyi, and the research shows that inorganic trace elements contained in the folium artemisiae argyi are active components for regulating blood.
At present, the quality of the folium artemisiae argyi can be evaluated by adopting the existing detection standards of the folium artemisiae argyi, such as the quality control industry standards of varieties or related preparations recorded in pharmacopoeia, existing patents and the like. Among them, patent document CN103705559A discloses a method for detecting ethyl acetate extract of artemisia argyi: the method comprises the steps of detecting main components of the folium artemisiae argyi extract by adopting an ultra-high liquid chromatography-mass spectrometry online analysis technology, constructing a folium artemisiae argyi extract fingerprint according to a detection result, and identifying the varieties of the folium artemisiae argyi and monitoring the quality of the folium artemisiae argyi extract by using the fingerprint and the technology thereof.
However, in the existing folium artemisiae argyi detection technology, the content of volatile components such as eucalyptol is often used as an index for folium artemisiae argyi detection, and the detection of the content of other volatile components and inorganic trace elements in the folium artemisiae argyi is not involved, so that the quality evaluation of the folium artemisiae argyi is incomplete, and the accuracy of the quality evaluation of the folium artemisiae argyi is affected. In addition, in the existing detection technology, the folium artemisiae argyi pretreatment process is complex.
Disclosure of Invention
The embodiment of the invention provides a quality evaluation method of folium artemisiae argyi, which is used for accurately and comprehensively evaluating the quality of the folium artemisiae argyi.
In order to solve the problems, the invention discloses a quality evaluation method of folium artemisiae argyi, which comprises the following steps:
measurement of the content of the main component of S1: weighing 0.8-1.2g of folium artemisiae argyi powder into a headspace bottle, adding 7-12ml of ultrapure water, sealing the headspace bottle, shaking uniformly, standing for 20-40min to obtain a test solution, preparing a reference solution, respectively measuring 1ml of headspace bottle gas of the reference solution and the test solution, injecting the headspace bottle gas into a gas chromatography-mass spectrometer to obtain a chromatogram-mass spectrogram, and analyzing the chromatogram-mass spectrogram to obtain the content of each main component in the folium artemisiae argyi;
measurement of inorganic element content of S2: weighing 0.15-0.35g of folium artemisiae argyi powder into a digestion tank, adding 8-10ml of nitric acid, standing overnight, digesting and dispelling acid, fixing the volume of digestion solution, shaking up, filtering to obtain an upper computer sample solution, and testing the upper computer sample solution by using an inductively coupled plasma mass spectrometer to obtain the content of each inorganic element in the folium artemisiae argyi;
s3 quality assessment: and performing quality evaluation on the folium artemisiae argyi according to the content of each main component and the content of each inorganic element in the folium artemisiae argyi to obtain a quality evaluation result.
In the invention, a headspace-gas chromatography-mass spectrometer is adopted to measure the content of main components (namely volatile components) in the folium artemisiae argyi. On one hand, the headspace bottle is adopted to carry out headspace sampling, so that the complex pretreatment process of the folium artemisiae argyi in the traditional folium artemisiae argyi detection method can be avoided, the detection flow of the folium artemisiae argyi can be simplified, the quality evaluation process of the folium artemisiae argyi is accelerated, and the pertinence and the practicability are good. On the other hand, the content of eucalyptol in the folium artemisiae argyi is measured, and the content of other volatile components in the folium artemisiae argyi, such as main components of caryophyllene, thujone, terpineol and the like, is also measured, so that the quality of the folium artemisiae argyi can be accurately evaluated.
In addition, the folium artemisiae argyi powder can be digested by the microwave digestion tank, and then the content of inorganic trace elements (such as heavy metal elements and other inorganic elements) in the folium artemisiae argyi is measured by the inductively coupled plasma mass spectrometer, so that the quality of the folium artemisiae argyi can be comprehensively evaluated by combining the content of main components and the content of the inorganic trace elements in the folium artemisiae argyi. In the specific implementation process, the contents of main components of folium artemisiae argyi, such as eucalyptol, thujone and caryophyllene, can be used as main quality control indexes, and the contents of inorganic trace elements in the folium artemisiae argyi, such as lead, cadmium, mercury, arsenic, copper, chromium, manganese and the like are combined to reflect the quality of the folium artemisiae argyi, so that the quality of the folium artemisiae argyi can be comprehensively and accurately evaluated.
Preferably, in step S1, the step of preparing the reference solution is: weighing eucalyptol, thujone, levocamphor and natural borneol, adding methanol for dissolving to obtain a mixed reference substance solution, weighing 800-.
According to the invention, eucalyptol, thujone, levocamphor and natural borneol can be selected to prepare the reference solution, so that the accurate measurement of the content of the main components in the folium artemisiae argyi can be realized according to the reference solution.
Preferably, in the step S1, the equilibrium temperature of the headspace bottle is 80-90 ℃;
the chromatographic conditions are as follows: 5% phenyl methyl polysiloxane as chromatographic column of fixed phase; keeping at 50 deg.C for 10min, and heating to 220 deg.C at 5 deg.C/min for 10 min; the temperature of a sample inlet is 240 ℃; the split ratio is 20: 1; the carrier gas is nitrogen.
Further preferably, in the step S1, the equilibrium temperature of the headspace bottle is 85 ℃.
Preferably, in step S1, the mass spectrum conditions are: adopting an EI source, wherein the temperature of an ion source is 230 ℃; the scanning method is full scanning, and the scanning mass number range is 30-500 m/z.
Preferably, in step S2, the sample solution is subjected to inductively coupled plasma mass spectrometry in a full-quantitative-semi-quantitative analysis mode.
In the invention, the analysis mode combining full quantification and semi-quantification can be adopted to carry out analysis on the folium artemisiae argyi23Na、27Al、39K、44Ca、47Ti、51V、54Fe、55Mn、56Fe、59Co、60Ni、65Cu、66Zn、71Ga、75As、78Se、85Rb、88Sr、95Mo、111Cd、114Cd、121Sb、137Ba、205Tl、208Pb waits for the measurement of the inorganic element content. Wherein, the full-quantitative and the semi-quantitative combination are adoptedThe analysis mode can avoid being influenced by the large content difference of each element in the folium artemisiae argyi sample, can accurately and quickly carry out quantitative analysis on each inorganic trace element in the folium artemisiae argyi, and further can accurately detect the content of each inorganic trace element in the folium artemisiae argyi. The method can collect all elements in the periodic table, namely all mass axes, and measure elements with higher concentration such as Na, Mg, K, Ca and other elements outside standard solutions by adopting a semi-quantitative analysis mode, thereby reducing the pollution of instruments, reducing the purchase of various element standard solutions and the complexity of preparing various elements one by one, having higher accuracy and precision and good stability and repeatability.
Further preferably, in step S2, when the full quantitative analysis mode is adopted, selecting is performed45Sc、72Ge、103Rh、115In、175Lu is used as an internal standard element for the inductively coupled plasma mass spectrometry.
In the invention, when the full quantitative analysis mode is adopted, an internal standard solution and a standard solution with a concentration gradient can be prepared in advance, mass spectrum detection is carried out on the internal standard solution and the standard solution with each concentration, a detection result is processed to obtain a standard curve (wherein the standard curve takes a measured value as a vertical coordinate and a concentration as a horizontal coordinate), mass spectrum detection is carried out on the on-machine sample solution, the detection result is inquired on the standard curve to obtain a corresponding concentration, then a blank test is carried out under the same analysis condition, and blank interference is deducted to accurately obtain the content of each inorganic element in the folium artemisiae argyi.
Particularly, when the full quantitative analysis mode is adopted for measurement, the method can be used for measuring45Sc as inorganic element to be measured52Cr、55Mn、56Internal standard element of Fe, will72Ge as63Cu、66Zn、75As、78Internal standard element of Se, is103Rh as95Internal standard element of Mo, the115In as111Cd、114Internal standard of Cd, and175lu as201Hg、202Hg、208Internal standard element of Pb.
Preferably, in step S2, before the digestion solution is fixed to volume, a step of adding a gold single element standard solution is further included.
In the invention, before the digestion solution is subjected to volume fixing, a proper amount of gold single element standard solution with the concentration of 1 mu g/ml can be added, and then water is added to fix the volume of the digestion solution.
Preferably, in the steps S1 and S2, the folium artemisiae argyi is pulverized to 50-90 meshes in advance to obtain the folium artemisiae argyi powder.
Further preferably, in the steps S1 and S2, the folium artemisiae argyi is pulverized to 65-80 meshes in advance to obtain the folium artemisiae argyi powder.
Compared with the prior art, the embodiment of the invention has the following advantages:
1. the method adopts the headspace-gas chromatography-mass spectrometer to measure the content of the main components in the folium artemisiae argyi, has high accuracy and precision, good stability and repeatability, can accurately and quickly carry out quantitative analysis, and is feasible and reliable in result.
2. The invention also adopts the inductively coupled plasma mass spectrometer to quantitatively measure the content of each inorganic element in the folium artemisiae argyi, the measuring method can accurately and quickly perform quantitative analysis of various inorganic elements without being influenced by large content difference of various inorganic elements in a sample, in addition, the semi-quantitative analysis mode can reduce instrument pollution, reduce purchase of various element standard solutions and complexity of preparing various elements one by one, simplify the detection process, have higher accuracy and precision and have good stability and repeatability.
3. In conclusion, the quality of the folium artemisiae argyi can be reflected by taking the contents of main components of the folium artemisiae argyi, such as eucalyptol, thujone, caryophyllene and the like as main quality control indexes and combining the contents of inorganic trace elements such as lead, cadmium, mercury, arsenic, copper, chromium, manganese and the like in the folium artemisiae argyi, so that the quality of the folium artemisiae argyi can be comprehensively and accurately evaluated.
Drawings
FIG. 1 is a semi-quantitative-full-quantitative detection profile of the standard solution of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Example 1
Measurement of the content of the main component of S1: the method adopts headspace-gas chromatography-mass spectrometry to carry out quantitative measurement on main components in the folium artemisiae argyi and comprises the following specific steps:
preparation of S11 test solution: pulverizing folium Artemisiae Argyi (such as south-positive folium Artemisiae Argyi) to powder, sieving with No. four sieve (65 mesh), mixing, precisely weighing 0.8g folium Artemisiae Argyi powder into 20ml headspace bottle, adding 7ml ultrapure water, sealing headspace bottle, shaking, and standing for 30min to obtain test solution.
Preparation of S12 control solution: precisely weighing reference substances including eucalyptol, thujone, levocamphor and natural borneol, adding methanol for dissolving, preparing into mixed reference substance solutions of 0.01, 0.02, 0.04, 0.1, 0.2 and 0.4mg/ml, measuring 1000ul of the mixed reference substance solutions into a 20ml headspace bottle, adding 10ml of water, sealing the headspace bottle, shaking uniformly, and standing for 30min to obtain the reference substance solution.
Wherein, the headspace parameters are: the equilibrium temperature was 85 ℃. Chromatographic conditions are as follows: adopting an HP-5MS chromatographic column and taking 5% phenyl methyl polysiloxane as a stationary phase of the chromatographic column; the temperature raising procedure is that the initial temperature is 50 ℃, the temperature is kept for 10 minutes, the temperature is raised to 220 ℃ at the rate of 5 ℃ per minute, and the temperature is kept for 10 minutes; the temperature of the detector is 250 ℃, and the temperature of the sample inlet is 240 ℃; split-flow sample injection with a split-flow ratio of 20: 1; the carrier gas was nitrogen and the flow rate was 1.0ml per minute. And (4) headspace sample injection, wherein the equilibrium temperature of a headspace bottle is 90 ℃, and the equilibrium time is 20 minutes. Mass spectrum conditions: the acquisition mode is full Scan (Scan); the scanning mass number range is 30.0-500.0 m/z; the threshold is 150.
S13 gas chromatography-mass spectrometry: respectively precisely measuring 1ml of headspace gas in the test solution and the reference solution in the steps S11 and S12, injecting the headspace gas into a gas chromatography-mass spectrometer, recording a chromatogram-mass spectrum, and calculating by peak area according to an external standard curve method to obtain the content of main components in the folium artemisiae argyi.
Measurement of the content of the main component of S2: measuring the content of inorganic elements in the folium artemisiae argyi by adopting microwave digestion-inductively coupled plasma mass spectrometry, and specifically comprising the following steps:
preparation of the machine sample solution of S21:
s211, sampling: pulverizing folium Artemisiae Argyi to pass through a five-mesh sieve (80 mesh), weighing 0.25g folium Artemisiae Argyi powder into a pressure-resistant high temperature-resistant microwave digestion tank, adding 8ml nitric acid, and standing overnight.
S212, microwave digestion: sealing and digesting by adopting the digestion program shown in the table 1, cooling the digestion solution to below 60 ℃ after complete digestion, taking out the digestion tank, and cooling. Digestion program as shown in table 1:
TABLE 1
S213 acid removal: taking out the digestion tank, placing the digestion tank in an acid removing device for removing acid, cooling the digestion solution to below 60 ℃ after the acid removing procedure is finished, taking out the digestion tank, and cooling.
S214, constant volume: transferring the digestion solution into a 50ml volumetric flask, washing the digestion tank for 3 times by using a small amount of water, merging washing liquids into the volumetric flask, adding 200 mu l of a gold single element standard solution (1 mu g/ml), diluting the solution to a scale by using water, shaking up the solution, and filtering the solution by using a 0.22 mu m (water system) filter membrane to obtain a machine sample solution.
Preparation of S22 standard solution: a proper amount of multi-element (Cr, Mn, Fe, Cu, Zn, As, Se, Mo, Cd and Pb) mixed standard stock solution is precisely measured, and diluted by 5% nitric acid solution to prepare mixed solutions with the series concentrations of 0ng, 0.5ng, 1ng, 2ng, 5ng, 10ng, 20ng, 50ng, 100ng, 200ng, 500ng and 1000ng per lm l. And precisely measuring a proper amount of mercury standard storage solution, and diluting with 5% nitric acid solution to prepare solutions containing 0ng, 0.2ng, 0.5ng, 1ng, 2ng, 5ng and 10ng of mercury per 1ml (the solution is prepared in an application way), so as to obtain the standard solution.
Preparation of internal standard solution of S23: precision measuring45Sc、72Ge、103Rh、115In、175Appropriate amount of Lu single element standard solution, 0.2% nitreDiluting with acid to obtain mixed solution containing 1 μ g of acid per lml to obtain internal standard solution.
The inductively coupled plasma mass spectrometry conditions are as follows: the collision pool mode is a He mode; the integration time is 0.100s-1.000 s; a full-quantitative-semi-quantitative analysis mode; the measurement was repeated 3 times; a conventional plasma mode; the isotope of the inorganic element to be detected is a full mass axis and a full periodic table element; the internal standard element is 1 mu g/ml45Sc、72Ge、103Rh、115In、175Lu。
S24 inductively coupled plasma mass spectrometry:
s241 full quantitative analysis mode:
will be provided with45Sc as inorganic element to be measured52Cr、55Mn、56Internal standard element of Fe, will72Ge as63Cu、66Zn、75As、78Internal standard element of Se, is103Rh as95Internal standard element of Mo, the115In as111Cd、114Internal standard of Cd, and175lu as201Hg、202Hg、208Internal standard element of Pb. The measured inorganic element may be corrected by using a correction equation according to the requirement of the instrument, which is not limited in the present invention. During measurement, an internal standard sample tube of the inductively coupled plasma mass spectrometer is always inserted into the internal standard solution in the instrument analysis working process, the sample tube of the inductively coupled plasma mass spectrometer is sequentially inserted into the standard solution with each concentration for measurement (the concentration is sequentially increased), and then a standard curve is drawn by taking the measured value (the average value of 3 readings) as the ordinate and the concentration as the abscissa; and inserting the sample tube of the inductively coupled plasma mass spectrometer into the upper computer sample solution, measuring, taking the average value of 3 readings, calculating the corresponding concentration from the standard curve, performing a blank test under the same analysis condition, and deducting blank interference.
S242 semi-quantitative analysis mode:
all elements in the periodic table, namely all mass axes, are collected, and elements with higher concentration, such as Na, Mg, K, Ca and other elements outside the standard solution, are measured by a semi-quantitative method.
And (3) measuring the folium artemisiae argyi powder by combining the full quantitative analysis mode in the step (S241) and the semi-quantitative analysis mode in the step (S242), so as to obtain the content of each inorganic element in the folium artemisiae argyi (wherein the detection map of the standard solution is shown in figure 1).
S3 quality assessment: and evaluating the quality of the folium artemisiae argyi according to the content of each main component in the folium artemisiae argyi measured in the step S1 and the content of each inorganic element in the folium artemisiae argyi measured in the step S2 so as to determine the quality grade of the folium artemisiae argyi.
In the embodiment of the invention, different evaluation indexes can be set for folium artemisiae argyi with different purposes, and based on the evaluation indexes, the quality of the folium artemisiae argyi is evaluated according to the content of main components and the content of inorganic elements in the folium artemisiae argyi to obtain a quality evaluation result; for example, if the mugwort leaves are mainly used for warming meridians and stopping bleeding, the mugwort leaves with high inorganic element content can be evaluated as superior mugwort leaves. The specific evaluation index may be set according to actual requirements, which is not limited in the embodiment of the present invention.
Example 2
The inventive example is essentially the same as example 1, with the following differences:
when the content of the main components is measured in step S1, in step S11, the mugwort leaves are pulverized in advance to pass through a No. four sieve (65 meshes), mixed uniformly, 1.0g of mugwort leaf powder is precisely weighed into a 20ml headspace bottle, 10ml of ultrapure water is added, the headspace bottle is sealed, shaken uniformly, and kept stand for 25min, so as to obtain a sample solution.
In the step S12, reference substances eucalyptol, thujone, levocamphor and natural borneol are precisely weighed, methanol is added for dissolution to prepare a mixed reference substance solution of 0.01, 0.02, 0.04, 0.1, 0.2 and 0.4mg/ml, 1000ul of the mixed reference substance solution is weighed to a 20ml headspace bottle, 10ml of water is added, the headspace bottle is sealed, shaking is carried out uniformly, and standing is carried out for 25min, so as to obtain the reference substance solution.
When the content of inorganic elements is measured in step S2, in step S211, the folium artemisiae argyi is pulverized to pass through a five-mesh sieve (i.e. 80 meshes), 0.2g of folium artemisiae argyi powder is weighed into a pressure-resistant high-temperature-resistant microwave digestion tank, 8ml of nitric acid is added, and the mixture is left to stand overnight.
Example 3
The inventive example is essentially the same as example 1, with the following differences:
when the content of the main components is measured in step S1, in step S11, the mugwort leaves are pulverized to pass through 70 meshes in advance, mixed uniformly, 1.0g of mugwort leaf powder is precisely weighed into a 20ml headspace bottle, 12ml of ultrapure water is added, the headspace bottle is sealed, shaken uniformly, and kept stand for 20min, so as to obtain a sample solution.
In the step S12, reference substances eucalyptol, thujone, levocamphor and natural borneol are precisely weighed, methanol is added for dissolution to prepare a mixed reference substance solution of 0.01, 0.02, 0.04, 0.1, 0.2 and 0.4mg/ml, 1200ul of the mixed reference substance solution is weighed into a 20ml headspace bottle, 13ml of water is added, the headspace bottle is sealed, shaking is carried out uniformly, and standing is carried out for 20min, so as to obtain the reference substance solution.
When the content of inorganic elements is measured in step S2, in step S211, the folium artemisiae argyi is pulverized to pass through a five-mesh sieve (i.e. 80 meshes), 0.15g of folium artemisiae argyi powder is weighed into a pressure-resistant high-temperature-resistant microwave digestion tank, 9ml of nitric acid is added, and the mixture is left to stand overnight.
Example 4
The inventive example is essentially the same as example 1, with the following differences:
when the content of the main components is measured in step S1, in step S11, the mugwort leaves are pulverized in advance to pass through a five-mesh sieve (i.e., 80 mesh), mixed uniformly, 1.2g of mugwort leaf powder is precisely weighed into a 20ml headspace bottle, 12ml of ultrapure water is added, the headspace bottle is sealed, shaken uniformly, and kept stand for 40min, so as to obtain a sample solution.
In the step S12, reference substances eucalyptol, thujone, levocamphor and natural borneol are precisely weighed, methanol is added for dissolution to prepare a mixed reference substance solution of 0.01, 0.02, 0.04, 0.1, 0.2 and 0.4mg/ml, 1200ul of the mixed reference substance solution is weighed into a 20ml headspace bottle, 8ml of water is added, the headspace bottle is sealed, shaking is carried out uniformly, and standing is carried out for 25min, so as to obtain the reference substance solution.
When the content of inorganic elements is measured in step S2, in step S211, the folium artemisiae argyi is pulverized to pass through a five-mesh sieve (i.e. 80 meshes), 0.3g of folium artemisiae argyi powder is weighed into a pressure-resistant high-temperature-resistant microwave digestion tank, 10ml of nitric acid is added, and the mixture is left to stand overnight.
Example 5
The inventive example is essentially the same as example 1, with the following differences:
when the content of the main components is measured in step S1, in step S11, the mugwort leaves are pulverized in advance to pass through a No. four sieve (65 meshes), mixed uniformly, 0.9g of mugwort leaf powder is precisely weighed into a 20ml headspace bottle, 8ml of ultrapure water is added, the headspace bottle is sealed, shaken uniformly, and kept stand for 25min, so as to obtain a sample solution.
In the step S12, reference substances eucalyptol, thujone, levocamphor and natural borneol are precisely weighed, methanol is added for dissolution to prepare a mixed reference substance solution of 0.01, 0.02, 0.04, 0.1, 0.2 and 0.4mg/ml, 800ul of the mixed reference substance solution is weighed into a 20ml headspace bottle, 15ml of water is added, the headspace bottle is sealed, shaking is carried out uniformly, and standing is carried out for 30min, so as to obtain the reference substance solution.
When the content of inorganic elements is measured in step S2, in step S211, the folium artemisiae argyi is pulverized to pass through a five-mesh sieve (i.e. 80 meshes), 0.35g of folium artemisiae argyi powder is weighed into a pressure-resistant high-temperature-resistant microwave digestion tank, 10ml of nitric acid is added, and the mixture is left to stand overnight.
Wherein, the detection results of the contents of the main components in the artemisia leaves of the examples 1 to 5 are shown in the table 2:
TABLE 2
Unit: mg/kg
As can be seen from table 2, the main components (i.e., volatile components) in the folium artemisiae argyi include eucalyptol, 4-terpineol, natural borneol, alpha-thujone, alpha-terpineol, levocamphor, L-carveol, beta-caryophyllene and the like, wherein the contents of beta-caryophyllene, 4-terpineol, natural borneol and the like are high.
Wherein, taking part of inorganic elements as an example, the detection results of the content of each inorganic element in the artemisia leaves of the examples 1-5 are shown in table 3:
TABLE 3
Unit: mg/kg
As is clear from Table 3, the above-mentioned moxa leaves are rich in the kinds of inorganic elements, and among them, K, Fe and the like are contained in a large amount. Because the folium artemisiae argyi contains more Fe element, the folium artemisiae argyi can be further proved to have the effect of warming meridians and stopping bleeding.
Performance test of S4 folium Artemisiae Argyi
S41 standard recovery test
Sampling and analyzing low, medium and high concentration standard sample solutions, and calculating the standard recovery rates of the low, medium and high concentration standard sample solutions of the components to be detected (such as eucalyptol, levocamphor, natural borneol and other main components, and Na, Mg, Al and other inorganic elements) in the folium artemisiae argyi.
The measurement method of the standard recovery rate comprises the following steps: taking two parts of the same folium artemisiae argyi sample solution, and adding a quantitative standard substance of the component to be detected into one part of the folium artemisiae argyi sample solution; the two samples are simultaneously detected according to the same analysis steps (specifically, refer to the detection method in embodiment 1 of the present invention), the detection result of the labeled folium artemisiae argyi sample solution (may be referred to as labeled sample measurement value) is subtracted by the detection result of the unlabeled folium artemisiae argyi sample solution (may be referred to as sample measurement value), and the ratio of the difference value to the theoretical value of the standard substance of the component to be detected (may be referred to as scalar value) is the labeled recovery rate of the component to be detected in folium artemisiae argyi: the recovery rate of spiked sample (spiked sample measurement value-sample measurement value) ÷ spiked amount × 100%.
The standard recovery rate of natural borneol in the folium artemisiae argyi sample solution is listed as follows, and is specifically shown in table 4:
from table 4, the standard recovery rate of natural borneol in folium artemisiae argyi is 92.80% -109.50%, so that the folium artemisiae argyi detection method has high accuracy in detecting the content of natural borneol.
It should be noted that, for simplicity of description, the method embodiments are described as a series of acts or combination of acts, but those skilled in the art will recognize that the present invention is not limited by the illustrated order of acts, as some steps may occur in other orders or concurrently in accordance with the embodiments of the present invention. Further, those skilled in the art will appreciate that the embodiments described in the specification are presently preferred and that no particular act is required to implement the invention.
The embodiments in the present specification are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
While preferred embodiments of the present invention have been described, additional variations and modifications of these embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the embodiments of the invention.
Finally, it should be further noted that, in the present document, the term "comprises/comprising" is intended to cover a non-exclusive inclusion, such that a process, a method, which comprises a series of elements, not only comprises those elements, but also comprises other elements not explicitly listed, or further comprises elements inherent to such a process, method. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in the processes or methods for which the element is included.
The method for evaluating the quality of the folium artemisiae argyi provided by the invention is described in detail, a specific example is applied in the method to explain the principle and the implementation mode of the invention, and the description of the example is only used for helping to understand the method and the core idea of the invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present invention.
Claims (10)
1. The quality evaluation method of the folium artemisiae argyi is characterized by comprising the following steps of:
measurement of the content of the main component of S1: weighing 0.8-1.2g of folium artemisiae argyi powder into a headspace bottle, adding 7-12ml of ultrapure water, sealing the headspace bottle, shaking uniformly, standing for 20-40min to obtain a test solution, preparing a reference solution, respectively measuring 1ml of headspace bottle gas of the reference solution and the test solution, injecting the headspace bottle gas into a gas chromatography-mass spectrometer to obtain a chromatogram-mass spectrogram, and analyzing the chromatogram-mass spectrogram to obtain the content of each main component in the folium artemisiae argyi;
measurement of inorganic element content of S2: weighing 0.15-0.35g of folium artemisiae argyi powder into a digestion tank, adding 8-10ml of nitric acid, standing overnight, digesting and dispelling acid, fixing the volume of digestion solution, shaking up, filtering to obtain an upper computer sample solution, and testing the upper computer sample solution by using an inductively coupled plasma mass spectrometer to obtain the content of each inorganic element in the folium artemisiae argyi;
s3 quality assessment: and performing quality evaluation on the folium artemisiae argyi according to the content of each main component and the content of each inorganic element in the folium artemisiae argyi to obtain a quality evaluation result.
2. The method for evaluating the quality of mugwort leaves according to claim 1, wherein the step of preparing the reference solution in step S1 comprises: weighing eucalyptol, thujone, levocamphor and natural borneol, adding methanol for dissolving to obtain a mixed reference substance solution, weighing 800-.
3. The method for evaluating the quality of mugwort leaves according to claim 1, wherein the equilibrium temperature of the headspace bottle in the step S1 is 80 to 90 ℃;
the chromatographic conditions are as follows: 5% phenyl methyl polysiloxane as chromatographic column of fixed phase; keeping at 50 deg.C for 10min, and heating to 220 deg.C at 5 deg.C/min for 10 min; the temperature of a sample inlet is 240 ℃; the split ratio is 20: 1; the carrier gas is nitrogen.
4. The method for evaluating the quality of mugwort leaves according to claim 3, wherein the equilibrium temperature of the headspace bottle in the step S1 is 85 ℃.
5. The method for evaluating the quality of mugwort leaves according to claim 1, wherein in the step S1, the mass spectrometry conditions are: adopting an EI source, wherein the temperature of an ion source is 230 ℃; the scanning method is full scanning, and the scanning mass number range is 30-500 m/z.
6. The method for evaluating the quality of mugwort leaves according to claim 1, wherein in step S2, the inductively coupled plasma mass spectrometry is performed on the above-mentioned sample solution in a full-quantitative-semi-quantitative analysis mode.
7. The method for evaluating the quality of mugwort leaf according to claim 6, wherein in the step S2, when the full quantitative analysis mode is adopted, the selection is performed45Sc、72Ge、103Rh、115In、175Lu is used as an internal standard element for the inductively coupled plasma mass spectrometry.
8. The method for evaluating the quality of mugwort leaves according to claim 1, further comprising a step of adding a aureolin standard solution before the digestion solution is fixed to volume in step S2.
9. The method for evaluating the quality of mugwort leaves according to claim 1, wherein the mugwort leaves are pulverized to 50-90 mesh in advance to obtain the mugwort leaf powder in the steps of S1 and S2.
10. The method for evaluating the quality of mugwort leaf according to claim 9, wherein the mugwort leaves are pulverized to 65-80 mesh in advance to obtain the mugwort leaf powder in the steps S1 and S2.
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