CN115561298A - Method for detecting content of rare earth elements in glabrous sarcandra herb - Google Patents
Method for detecting content of rare earth elements in glabrous sarcandra herb Download PDFInfo
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- CN115561298A CN115561298A CN202211150299.XA CN202211150299A CN115561298A CN 115561298 A CN115561298 A CN 115561298A CN 202211150299 A CN202211150299 A CN 202211150299A CN 115561298 A CN115561298 A CN 115561298A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
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- 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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- 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
- G01N1/40—Concentrating samples
- G01N1/4055—Concentrating samples by solubility techniques
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- 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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
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- 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
- G01N1/40—Concentrating samples
- G01N1/4055—Concentrating samples by solubility techniques
- G01N2001/4061—Solvent extraction
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention discloses a method for detecting the content of rare earth elements in glabrous sarcandra herb, which comprises the following steps: preparing a sample, (2) preparing a standard solution, (3) drawing a standard curve, and (4) measuring the content of the rare earth element. The invention firstly uses cellulase to hydrolyze and then carries out supercritical CO 2 After a sample solution is obtained by fluid extraction, the content of 16 rare earth elements in the glabrous sarcandra herb is determined by adopting an inductively coupled plasma mass spectrometry method, the detection method is simple and rapid, the repeatability is good, the detection requirement can be met, and certain basic data and scientific basis are provided for the quality control and pharmacological research of the glabrous sarcandra herb.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicine detection, in particular to a method for detecting the content of rare earth elements in glabrous sarcandra herb.
Background
Glabrous Sarcandra herb, also known as Guanyin tea, elderberry, sarcandra glabra and the like, is a dried whole plant of Sarcandra glabra (Thunb.) Nakai of chloranthaceae, has the effects of clearing heat and cooling blood, promoting blood circulation and removing spots, and dispelling wind and dredging collaterals, and is mainly used for treating blood heat, macula and eruption, rheumatic arthralgia, traumatic injury and other symptoms. Glabrous sarcandra herb is mainly distributed in the south areas of the Yangtze river such as Guangxi, yunnan, guizhou and Jiangxi in China, and is a characteristic whole-grass Chinese herbal medicine in the south of Lingnan. Modern pharmacological research shows that the glabrous sarcandra herb mainly has various pharmacological effects of resisting bacteria, diminishing inflammation, resisting tumors, resisting cancers, inhibiting platelet reduction, relieving asthma, eliminating phlegm and the like, and is a good medicinal and edible Chinese herbal medicine in the prescription of minority nationalities. Related researches find that the glabrous sarcandra herb and the extract thereof have wide pharmacological action, definite medicinal effect and good safety, are main raw materials of dozens of traditional Chinese medicine preparations such as glabrous sarcandra herb injection, sarcandra glabra buccal tablets, sarcandra glabra anti-tumor injection and the like, and are also main components of related foods and cosmetics such as sarcandra glabra chewing gum, sarcandra glabra tea bags, sarcandra glabra toothpaste, coral facial cleanser and the like. Therefore, the glabrous sarcandra herb is a Chinese medicinal material which is worthy of being deeply developed and utilized, and has wide development prospect in the fields of medicines, foods, health-care products and the like.
At present, most of researches on effective components of glabrous sarcandra herb are concentrated on organic compounds such as coumarins, flavonoids, sesquiterpenes, organic acids and polysaccharides, and researches on rare earth elements in the glabrous sarcandra herb are not reported. The related research shows that the rare earth element as one of the inorganic elements can not only improve the yield and the quality of the medicinal materials, but also improve the curative effect of the Chinese herbal medicine because the rare earth element contained in the medicinal materials has a close relationship with the exertion of the medicinal effect, so the research on the inorganic elements contained in the Chinese herbal medicine is more and more emphasized by people. The method adopts an inductively coupled plasma mass spectrometry to detect and quantitatively analyze 16 rare earth elements including Sc, Y, la, ce, pr, nd, sm, eu, gd, tb, dy, ho, er, tm, yb and Lu in the glabrous sarcandra herb medicinal material, and performs multivariate statistical analysis on the measurement result so as to provide a certain reference for the deep development of the glabrous sarcandra herb medicinal material.
Disclosure of Invention
The invention aims to provide a method for detecting the content of rare earth elements in glabrous sarcandra herb, thereby solving the problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme: a method for detecting the content of rare earth elements in glabrous sarcandra herb comprises the following steps:
(1) Preparing a test article: drying and crushing herba Pileae Scriptae, performing enzymolysis with cellulase, and subjecting the herba Pileae Scriptae after enzymolysis to supercritical CO 2 Extracting the fluid, combining the obtained extract in a volumetric flask, finally, holding to a scale and shaking up to obtain a test solution;
(2) Preparing a standard solution: taking a proper amount of various rare earth element standard solutions, adding nitric acid for dilution to prepare mixed standard solutions containing various elements, taking Rh solution as an internal standard element, and storing for later use;
(3) Drawing a standard curve: taking the standard solution, carrying out linear relation measurement under the working condition of ICP-MS, and drawing a standard curve by taking the ratio of mass concentration to internal standard element as a horizontal coordinate and the absorbance value as a vertical coordinate;
(4) Determination of rare earth element content: and measuring the content of the rare earth element in the test solution by adopting ICP-MS under the working condition.
Preferably, the specific process of the enzymatic hydrolysis by the cellulase is as follows: weighing 0.1-1g of pulverized glabrous sarcandra herb granules, and performing enzymolysis on the glabrous sarcandra herb granules for 2-5h by using 50-100mL of cellulase solution.
Preferably, the supercritical CO 2 The conditions of the fluid extraction were: the extraction pressure is 10-25MPa, the extraction temperature is 35-45 ℃, and CO is added 2 The flow rate is 3-5L/min.
Preferably, the various types of rare earth element standard solutions comprise Sc, Y, la, ce, pr, nd, sm, eu, gd, tb, dy, ho, er, tm, yb and Lu standard solutions.
Preferably, 2% nitric acid is added into various rare earth element standard solutions to be diluted into mixed standard solutions containing 1, 2, 5, 10 and 20 mu g/L of each element, 20 mu g/L Rh solution is used as an internal standard element, and the mixed standard solutions are stored at 4 ℃ for later use.
Preferably, in steps (3) and (4), the operating conditions of the ICP-MS are plasma rf power: 1200W; the flow rate of the atomizer, the flow rate of the plasma and the flow rate of the auxiliary gas are respectively 0.88L/min, 0.88L/min and 1.20L/min; deflection plate voltage: -12.0V.
Compared with the prior art, the invention has the following beneficial effects:
the method for detecting the content of the rare earth elements in the glabrous sarcandra herb provided by the invention comprises the steps of firstly performing cellulose enzymolysis and then performing supercritical CO (carbon dioxide) hydrolysis 2 After a sample solution is obtained by fluid extraction, the content of 16 rare earth elements in the glabrous sarcandra herb is determined by adopting an inductively coupled plasma mass spectrometry method, the detection method is simple and rapid, the repeatability is good, the detection requirement can be met, and certain basic data and scientific basis are provided for the quality control and pharmacological research of the glabrous sarcandra herb.
Drawings
FIG. 1 shows the distribution characteristics of the rare earth element in glabrous sarcandra herb.
FIG. 2 shows the distribution of total rare earth, light rare earth and heavy rare earth in the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1
A method for detecting the content of rare earth elements in glabrous sarcandra herb comprises the following steps:
(1) Preparing a test article: drying and crushing glabrous sarcandra herb, weighing 0.1g of crushed glabrous sarcandra herb particles, and carrying out enzymolysis on the glabrous sarcandra herb particles for 2 hours by using 50mL of cellulase solution; then passing the herba Pileae Scriptae after enzymolysis through supercritical CO 2 Extracting with fluid at 35 deg.C and 10MPa for CO 2 The flow rate is 3L/min; mixing the obtained extractive solutions in a volumetric flask, and finally, adding to scale and shaking to obtain a sample solution;
(2) Preparing a standard solution: taking a proper amount of standard solutions of Sc, Y, la, ce, pr, nd, sm, eu, gd, tb, dy, ho, er, tm, yb and Lu, adding 2% nitric acid to dilute the standard solutions to prepare mixed standard solutions containing 1, 2, 5, 10 and 20 mu g/L of each element, taking 20 mu g/L Rh solution as an internal standard element, and storing the internal standard solution at 4 ℃ for later use;
(3) Drawing a standard curve: taking the standard solution, carrying out linear relation measurement under the working condition of ICP-MS, and drawing a standard curve by taking the ratio of mass concentration to internal standard element as a horizontal coordinate and the absorbance value as a vertical coordinate;
(4) Determination of rare earth element content: and measuring the content of the rare earth element in the test solution by adopting ICP-MS under the working condition.
The working conditions of the ICP-MS are plasma radio frequency power: 1200W; the flow rate of the atomizer, the flow rate of the plasma and the flow rate of the auxiliary gas are respectively 0.88L/min, 0.88L/min and 1.20L/min; deflection plate voltage: -12.0V.
Example 2
Other process parameters of the present embodiment are the same as those of embodiment 1, except that: (1) preparing a test article: drying and crushing glabrous sarcandra herb, weighing 1g of crushed glabrous sarcandra herb particles, and performing enzymolysis on the glabrous sarcandra herb particles for 5 hours by using 100mL of cellulase solution; then passing the herba Pileae Scriptae after enzymolysis through supercritical CO 2 Extracting with fluid at 25MPa and 45 deg.C under CO 2 The flow rate is 5L/min; mixing the obtained extractive solutions in a volumetric flask, and finally, adding to scale and shaking to obtain the sample solution.
1. The linear regression equation, correlation coefficient, detection limit, and quantitative limit of each rare earth element obtained by the detection method of example 1 are shown in table 1. As can be seen from Table 1, the standard curves of the elements have good linear relationship, and r is greater than 0.999.
TABLE 1 examination of the Linear relationship of elements
2. Then carrying out tests on the detection method such as precision, repeatability, stability and the like
(1) Precision test
And (3) sucking the same mixed standard solution, continuously injecting samples for 6 times respectively according to the working conditions of the instrument under the item of 1.3.2, measuring the response signal values of 16 rare earth elements, and calculating the RSD value of the rare earth elements. The results show that the RSD is less than 3.0 percent, which indicates that the precision of the instrument is good.
(2) Repeatability test
Taking the same glabrous sarcandra herb sample, preparing a test solution according to the method under the item '1.3.1', then measuring according to the condition of the item '1.3.2', calculating the content of each rare earth element, calculating the RSD value, and carrying out parallel operation for 6 times. The result shows that the RSD value of each element is less than 5.0 percent, which indicates that the method has good repeatability and can meet the detection requirement.
(3) Stability test
Weighing a glabrous sarcandra herb sample, preparing a test solution according to the item '1.3.1', respectively measuring for 0 hour, 2 hours, 4 hours, 8 hours, 16 hours and 24 hours, calculating the content of each rare earth element in the sample, and obtaining the RSD value of less than 4.0%, which indicates that the test solution has good stability within 24 hours.
(4) Sample recovery rate
And (3) adding the measured glabrous sarcandra herb sample into the mixed reference solution, preparing a test solution, measuring the content of each element by using ICP-MS (inductively coupled plasma-mass spectrometry), and calculating the recovery rate. The result shows that the sample recovery rate of each rare earth element is 88.6-115.3%, and the RSD is less than 5.0%, which indicates that the method has good accuracy.
3. Data processing
Data statistics and correlation analysis, mapping, etc. were performed using Microsoft Excel 22019, SPSS 21.7, and Origin 2018 software.
4. Determination result of content of rare earth elements in glabrous sarcandra herb
After each batch of glabrous sarcandra herb samples are treated according to the method under the item 1.3.1, the content of 16 rare earth elements in the samples is measured according to the measurement conditions under the item 1.3.2, the data of each sample is read 3 times, and the average value is taken, and the specific results are shown in table 2 and figure 1.
TABLE 2 determination of rare earth elements in glabrous sarcandra herb materials (mg/kg)
As can be seen from Table 2, the average content of Ce element among the 16 rare earth elements tested is the highest, which reaches 3.1366mg/kg; secondly, la and Nd elements with the average content of 1.2956 and 1.0178mg/kg; the contents of other elements are all lower than 1.0mg/kg, wherein the average content of the elements Y & gtSc & gtPr & gtSm & gtGd & gtDy is between 0.1 and 1.0mg/kg, the elements Er & gtEu & gtYb & gtTb & gtHo are relatively less, the average content is between 0.02 and 0.07mg/kg, the content of the elements Tm & gtLu is extremely low, and the average content is lower than 0.01mg/kg.
As shown in FIG. 1, the content of rare earth elements in herba Pileae Scriptae conforms to the Oddo-Harkins law (even rule) [15] That is, the content of the even atomic number element is greater than that of the odd atomic number element, and the content distribution of the rare earth elements between different batches of samples has certain similarity. The commonality is hopeful to be used for distinguishing the glabrous sarcandra herb from other medicinal materials and provides a certain reference for tracing and identifying the glabrous sarcandra herb.
5. Distribution of total rare earth, light rare earth and heavy rare earth
The content analysis was performed from the perspective of the total amount of rare earth, light rare earth (La, ce, pr, nd, sm, eu) and heavy rare earth (Sc, Y, gd, tb, dy, ho, er, tm, yb, lu), and the results are shown in FIG. 2. As shown in FIG. 2, the total content of rare earth elements in the glabrous sarcandra herb is 3.2265-11.1057 mg/kg, and the average content is 7.4146mg/kg; the content of the light rare earth elements is (La, ce, pr, nd, sm and Eu) 2.5413-8.9199 mg/kg, and the average content is 5.9823mg/kg; the content of heavy rare earth elements (Sc, Y, gd, tb, dy, ho, er, tm, yb and Lu) is 0.6852-2.2774 mg/kg, and the average content is 1.4323mg/kg. And the rare earth element composition in the medicinal materials has obvious regularity, namely the content of light rare earth elements is far higher than that of heavy rare earth elements.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. A method for detecting the content of rare earth elements in glabrous sarcandra herb is characterized by comprising the following steps:
(1) Preparing a test article: drying and pulverizing herba Pileae Scriptae, performing enzymolysis with cellulase, and subjecting the herba Pileae Scriptae after enzymolysis to supercritical CO 2 Extracting the fluid, combining the obtained extract in a volumetric flask, finally, holding to a scale and shaking up to obtain a test solution;
(2) Preparing a standard solution: taking a proper amount of various rare earth element standard solutions, adding nitric acid for dilution to prepare mixed standard solutions containing various elements, taking Rh solution as an internal standard element, and storing for later use;
(3) Drawing a standard curve: taking the standard solution, carrying out linear relation measurement under the working condition of ICP-MS, and drawing a standard curve by taking the ratio of mass concentration to internal standard element as a horizontal coordinate and the absorbance value as a vertical coordinate;
(4) Determination of rare earth element content: and measuring the content of the rare earth element in the test solution by adopting ICP-MS under the working condition.
2. The method for detecting the content of rare earth elements in glabrous sarcandra herb according to claim 1, wherein: the specific process of enzymolysis of the cellulase is as follows: weighing 0.1-1g of pulverized glabrous sarcandra herb granules, and performing enzymolysis on the glabrous sarcandra herb granules for 2-5h by using 50-100mL of cellulase solution.
3. The method for detecting the content of rare earth elements in glabrous sarcandra herb according to claim 1, wherein: the supercritical CO 2 The conditions of the fluid extraction were: the extraction pressure is 10-25MPa, the extraction temperature is 35-45 ℃, and CO is added 2 The flow rate is 3-5L/min.
4. The method for detecting the content of rare earth elements in glabrous sarcandra herb according to claim 1, wherein: the various rare earth element standard solutions comprise Sc, Y, la, ce, pr, nd, sm, eu, gd, tb, dy, ho, er, tm, yb and Lu standard solutions.
5. The method for detecting the content of rare earth elements in glabrous sarcandra herb according to claim 4, wherein: adding 2% nitric acid into various rare earth element standard solutions to dilute and prepare mixed standard solutions containing 1, 2, 5, 10 and 20 mu g/L of each element, using 20 mu g/L Rh solution as an internal standard element, and storing at 4 ℃ for later use.
6. The method for detecting the content of rare earth elements in glabrous sarcandra herb according to claim 1, wherein: in the steps (3) and (4), the working condition of the ICP-MS is that the plasma radio frequency power is as follows: 1200W; the flow rate of the atomizer, the flow rate of the plasma and the flow rate of the auxiliary gas are respectively 0.88L/min, 0.88L/min and 1.20L/min; deflection plate voltage: -12.0V.
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| CN116735514A (en) * | 2023-08-11 | 2023-09-12 | 昆明理工大学 | Method for rapidly detecting gastrodia elata sulfuration markers by nano-enzyme combined liquid-liquid microextraction |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116735514A (en) * | 2023-08-11 | 2023-09-12 | 昆明理工大学 | Method for rapidly detecting gastrodia elata sulfuration markers by nano-enzyme combined liquid-liquid microextraction |
| CN116735514B (en) * | 2023-08-11 | 2023-11-03 | 昆明理工大学 | Method for rapidly detecting gastrodia elata sulfuration markers by nano-enzyme combined liquid-liquid microextraction |
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