CN118275573A - Method for measuring content of sandalwood medicinal materials, decoction pieces, standard decoction and formula particles - Google Patents
Method for measuring content of sandalwood medicinal materials, decoction pieces, standard decoction and formula particles Download PDFInfo
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- 239000012488 sample solution Substances 0.000 claims abstract description 32
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- 239000000243 solution Substances 0.000 claims description 56
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- Medicines Containing Plant Substances (AREA)
Abstract
The invention provides a method for measuring the content of sandalwood medicinal materials, decoction pieces, standard decoction and prescription particles, which takes acteoside as a reference substance, and takes acetonitrile-water with the volume ratio of (15-20) to (80-85) as a mobile phase through liquid chromatography detection of a sample solution and a reference substance solution.
Description
Technical Field
The invention belongs to the technical field of medicine detection, and particularly relates to a method for measuring the content of sandalwood medicinal materials, decoction pieces, standard decoction and formula particles.
Background
The history of the sandalwood is long, and the sandalwood is recorded as a lower product by the book of the Chinese herbal medicine in the Han dynasty, namely, the purple sandalwood, but the sandalwood is now a generic name of plants in the genus santalum, and is not the currently used sandalwood, and is recorded in the book of the Ming's medicine: salty taste and slightly cold taste. It is mainly used for treating malignant toxin and wind toxin. And "promoting qi circulation, warming middle-jiao, stimulating appetite and relieving pain" recorded in modern pharmacopoeia. Can be used for treating stagnation of qi due to cold, chest distress, chest pain, abdominal pain, emesis, and anorexia. "have something in and out". "white sandalwood" is described in Ben early Chan mu: pungent, warm and nontoxic. "," Pterocarpus Indicus: salty, slightly cold, nontoxic. The description of the red sandalwood is consistent with the description of the Ming Yi Bie Ji, and the description of the white sandalwood is consistent with the taste of the 2020 edition of the modern Chinese pharmacopoeia. The following is loaded: "Santalum album: pungent and warm. Regulate spleen and lung. Induce the chest and diaphragm to promote. Treating dysphagia. To relieve pain in the heart and abdomen. And the insect killing agent can be used for killing the insect. Stimulating appetite. It is also basically consistent with the nature, taste and function of the edition 2020 of Chinese pharmacopoeia.
The current examination proves that the mixed use condition of the sandalwood, the red sandalwood and the yellow sandalwood does exist. At present, little research is needed in the aspect of sandalwood content measurement, and in order to evaluate and control the quality of sandalwood as a whole, a unified method for measuring the content of sandalwood needs to be established.
Disclosure of Invention
Therefore, the invention aims to provide a method for measuring the content of sandalwood medicinal materials, decoction pieces, standard decoction and prescription particles.
In order to achieve the purpose, the invention adopts the following technical scheme:
The invention provides a method for measuring the content of sandalwood medicinal materials, decoction pieces, standard decoction and prescription particles, which comprises the following steps:
measuring the reference substance solution and the sample solution by liquid chromatography;
The reference substance in the reference substance solution is acteoside;
the conditions of the liquid chromatography are as follows: acetonitrile-water is used as a mobile phase, and the volume ratio of acetonitrile to water in the acetonitrile-water is (15-20) (80-85).
More preferably, the volume ratio of acetonitrile to water in the acetonitrile-water is (17-19): (81-83).
Preferably, the sample solution is obtained by mixing the sample with 30 to 80vol% methanol and extracting.
Preferably, the sample solution is obtained by mixing the sample with 50vol% methanol and extracting.
Preferably, the mass volume ratio of the test sample to 30-80 vol% of methanol is 1 (100-500).
Preferably, the mass volume ratio of the test sample to 50vol% methanol is 1 (100-500).
Preferably, the extraction time is not less than 30min.
Preferably, the reference solution is obtained by mixing the acteoside with 30-80 vol% of methanol and extracting.
Preferably, the concentration of the acteoside in the reference solution is 1-384 mug/mL.
Preferably, the addition amounts of the control solution and the test solution are each independently selected from 8 to 12. Mu.L.
More preferably, the addition amounts of the control solution and the test solution are 10 μl.
Preferably, the filler of the chromatographic column in the liquid chromatography is octadecylsilane chemically bonded silica.
Preferably, the theoretical plate number of the chromatographic column is not less than 3000 calculated as acteoside peak.
Preferably, the detection wavelength of the liquid chromatograph is 300-340 nm.
Compared with the prior art, the invention has the beneficial effects that:
The invention provides a method for measuring the content of sandalwood medicinal materials, decoction pieces, standard decoction pieces and formula particles, which takes acteoside as a reference substance, and the result shows that the method can scientifically identify the sandalwood medicinal materials, decoction pieces, standard decoction pieces and formula particles, can control the internal quality of the sandalwood and related preparations on the whole and macroscopically, can effectively ensure the curative effect of the medicaments, and ensures that the medicinal materials and related preparations are controlled in a more regular quality.
Through verification, the method can effectively separate and measure the acteoside components of the sandalwood medicinal materials, decoction pieces, standard decoction pieces and formula particles, can effectively ensure the uniformity and stability of the quality of the sandalwood medicinal materials, decoction pieces, standard decoction pieces and formula particles, and provides guidance for the quality control of the sandalwood. The method provided by the invention has the advantages of comprehensive detection, simplicity and convenience in operation, good stability, high precision, good repeatability and easiness in mastering.
Drawings
FIG. 1 is an ultraviolet absorption spectrum of acteoside;
FIG. 2 is a view of the sandalwood formulation as a test sample in different mobile phases;
FIG. 3 is a chromatogram obtained by performing specificity investigation by taking sandalwood formula particles as a test sample;
FIG. 4 is a standard graph of acteoside.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention, and it is apparent 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.
Aiming at the problem that a unified method for measuring the content of the sandalwood is lacking in the prior art, the invention provides a method for measuring the content of sandalwood medicinal materials, decoction pieces, standard decoction and formula particles, which comprises the following steps:
measuring the reference substance solution and the sample solution by liquid chromatography;
The reference substance in the reference substance solution is acteoside.
In the invention, the sample solution is the solution of the sandalwood medicinal materials, decoction pieces, standard decoction and formula particles, and the sandalwood medicinal materials, decoction pieces, standard decoction and formula particles are the samples.
In the invention, the preparation methods of different samples are explored and established, and the exploratory factors mainly comprise selection of extraction solvents, investigation of extraction time and investigation of addition amount of the extraction solvents in the preparation process of different sample solutions.
In some embodiments of the invention, the test solution is generally obtained from the test after mixing with 30 to 80vol% methanol, preferably 50vol% methanol, and extracting. In the present invention, the extraction method may be reflux extraction or ultrasonic extraction, and is not particularly limited. In order to ensure the thoroughness of the extracted active ingredient, it is preferable that the time of the reflux extraction or ultrasonic extraction is not less than 30 minutes. Wherein, the amount of the sample is 1g, and the addition amount of the extraction solvent may be 100-500 mL, and may be 100mL, 150mL, 200mL, 250mL, 300mL, 350mL, 400mL, 450mL, 500mL, or the like.
It should be noted that when the extraction mode is ultrasonic extraction, the power of ultrasonic extraction in the present invention is preferably 500 to 700W, more preferably 600W, and the frequency is preferably 30 to 50kHz, more preferably 40kHz.
In some embodiments of the invention, when the test is a sandalwood formulation, the test solution is prepared according to the following method:
Taking a proper amount of the product (namely, sandalwood formula particles), grinding, taking about 0.1g, precisely weighing, placing into a conical bottle with a plug, precisely adding 50mL of 50vol% methanol, sealing, weighing, performing ultrasonic treatment (power 600W, frequency 40 kHz) for 30min, cooling, weighing again, supplementing the lost weight with 50vol% methanol, shaking uniformly, filtering, and taking the subsequent filtrate.
In some embodiments of the invention, when the test is a santalum, the test solution is prepared as follows:
Taking about 0.5g of the product, (sieving with a third sieve), precisely weighing, placing in a conical flask with a plug, precisely adding 50mL of 50vol% methanol solution, sealing, weighing, performing ultrasonic treatment (power 600W, frequency 40 kHz) for 30min, cooling, weighing again, supplementing the lost weight with 50vol% methanol solution, shaking uniformly, filtering, and taking subsequent filtrate.
In some embodiments of the invention, when the test article is a santalum decoction piece, the test article solution is prepared according to the following method:
Taking about 0.5g of the product, (sieving with a third sieve), precisely weighing, placing in a conical flask with a plug, precisely adding 50mL of 50vol% methanol solution, sealing, weighing, performing ultrasonic treatment (power 600W, frequency 40 kHz) for 30min, cooling, weighing again, supplementing the lost weight with 50vol% methanol solution, shaking uniformly, filtering, and taking subsequent filtrate.
In some embodiments of the invention, when the test is a standard decoction of sandalwood, the test solution is prepared according to the following method:
About 0.1g of the product powder is precisely weighed, placed in a conical bottle with a plug, precisely added with 50mL of 50vol% methanol solution, sealed, weighed, subjected to ultrasonic treatment (power 600W and frequency 40 kHz) for 30min, cooled, weighed again, complemented with 50vol% methanol solution, shaken uniformly, filtered, and the subsequent filtrate is taken, thus obtaining the product.
In the invention, the reference substance in the reference substance solution is acteoside. The compounds which are separated from the sandalwood medicinal materials at present are mainly sesquiterpenes. In addition, the composition also comprises various chemical components such as monoterpenes, lignans and the like, wherein sesquiterpenes and monoterpenes are lipophilic components. Most of the current researches are limited on lipophilic components, 50vol% of methanol is selected for researching the hydrophilic and lipophilic components, and the development of chromatographic conditions indicates that the acteoside belongs to phenethyl alcohol glycoside compounds, is a compound with relatively high content. Therefore, the experiment can better mine the medicinal value of the sandalwood by screening and specifically selecting the acteoside as the content measurement index of the sandalwood.
In some embodiments of the invention, the control solution is obtained by extraction after mixing the acteoside with 30 to 80vol% methanol, preferably 50vol% methanol. The extraction mode refers to the preparation of the sample solution.
According to linear investigation, the concentration of the acteoside in the control solution is preferably 1-384 mug/mL, more preferably 5-300 mug/mL, so that the obtained acteoside linear curve can show good linear relation.
After the sample solution and the reference solution are obtained according to the method, the invention carries out liquid chromatography determination on the reference solution and the sample solution. It should be noted that not all mobile phases involved in liquid chromatography can obtain good detection results, and the invention adopts different mobile phases for research, so that the result shows that the chromatographic peak type obtained by acetonitrile-water under the condition of isocratic elution is relatively complete, and the chromatographic column is friendly, so that the acetonitrile-water is used as the mobile phase of the chromatographic determination method. Wherein the volume ratio of acetonitrile to water in the acetonitrile-water is preferably (15-20): (80-85), more preferably (17-19): (81-83), and most preferably 19:81.
The invention uses full-wave spectrum collection to the calycosin reference substance solution, and uses the analysis of the spectrum to determine that the optimal detection wavelength for determining the content of the calycosin is preferably 300-340 nm, more preferably 330nm.
The invention establishes liquid chromatographic conditions through liquid chromatographic conditions and system adaptability tests as follows:
Octadecylsilane chemically bonded silica is used as a filler (column length is 250mm, inner diameter is 4.6mm, and particle diameter is 5 μm); acetonitrile-water solution (the volume ratio of acetonitrile to water is (15-20): 80-85)) is taken as a mobile phase; the detection wavelength is 300-340 nm. The number of theoretical plates should be not less than 3000 calculated according to acteoside peak.
In the present invention, the specific measurement method is as follows:
Precisely sucking 8-12 μl of each of the control solution and the sample solution, preferably 10 μl, and injecting into a liquid chromatograph, and measuring under the above liquid chromatography conditions.
After the preparation method of the sample solution and the liquid chromatography measuring method are determined, the method is also subjected to methodology investigation aiming at the liquid chromatography measuring method, and the method mainly comprises specificity experiments, precision investigation, repeatability investigation, intermediate precision investigation (different instrument investigation and different personnel time investigation), linear investigation, stability investigation, accuracy investigation, durability investigation and the like.
In the specificity investigation, the negative solution and the reference solution and the sample solution need to be subjected to liquid chromatography detection together. In the present invention, the negative solution is a solvent prepared after the sample of sandalwood is not added, and the addition amount thereof is 8 to 12. Mu.L, preferably 10. Mu.L. The result shows that the chromatogram of the negative solution has no interference to the measurement of the peak to be measured, and the specificity of the method is good.
Further, after the inspection is completed, a series of verification of multiple batches of samples is performed according to the liquid chromatography determination method, and the result shows that the method can effectively separate and determine the acteoside components of the sandalwood medicinal materials, decoction pieces, standard decoction pieces and formula particles, effectively ensure the uniformity and stability of the quality of the sandalwood medicinal materials, decoction pieces, standard decoction pieces and formula particles, and provide guidance for the quality control of the sandalwood.
In order to further illustrate the present invention, the following examples are provided. The experimental materials used in the following examples of the present invention are all generally commercially available. The "%" referred to below, unless otherwise specified, represent volume percent.
Example 1
1 Laboratory apparatus and materials
Instrument 1 (zemoeid), instrument 2 (agilent 1260), instrument 3 (shimadzu LC-20);
An electronic balance: ME204E/02, MS205D M, XP26 (Metrele Tolyduo instruments Co., ltd.);
Ultrapure water machine: cell type 1810A (Shanghai mueller scientific instruments limited);
ultrasonic cleaner: KQ5200DB model (600W, 40KHz; kunshan ultrasonic instruments Co., ltd.);
Chromatographic column: column 1 (TC-C18), column 2 (SB-C18), column 3 (extension-C18);
Acetonitrile, phosphoric acid, methanol and formic acid are chromatographic purity; the water is ultrapure water, and other reagents are all analytically pure;
Acteoside (acteoside) reference (Chinese food and drug assay institute, lot number: 111530-201914, content of 95.2%);
sandalwood formula particles: TX-01, TX-02, TX-03, TX-04 and TX-05 are provided by Sichuan New green pharmaceutical industry technology development Co., ltd;
Sandalwood medicinal material: TX-YC-01, TX-YC-02, TX-YC-03, TX-YC-04 and TX-YC-05, provided by Sichuan New green pharmaceutical technology development Co., ltd;
sandalwood decoction pieces: TX-YP-01, TX-YP-02, TX-YP-03, TX-YP-04, TX-YP-05, supplied by Sichuan New green pharmaceutical technology development Co., ltd;
sandalwood standard decoction: TX-BT-01, TX-BT-02, TX-BT-03, TX-BT-04 and TX-BT-05 are provided by Sichuan New Green pharmaceutical technology development Co.
2 Establishment of formula particle content determination method
2.1 Sandalwood formula particles
2.1.1 Preparation of sample solutions
Taking a proper amount of the product, grinding, taking about 0.1g, precisely weighing, placing into a conical flask with a plug, precisely adding 50mL of 50% methanol, sealing, weighing, performing ultrasonic treatment (power 600W, frequency 40 kHz) for 30min, cooling, weighing again, supplementing the lost weight with 50% methanol, shaking uniformly, filtering, and taking the subsequent filtrate.
2.1.2 Preparation of control solution
Taking a proper amount of the calycosin reference substance, precisely weighing, and adding 50% methanol solution to prepare a solution containing 40 mug per 1 mL.
2.1.3 Preparation of negative solutions
Taking proper amount of auxiliary materials, taking about 0.1g, precisely weighing, placing into a conical bottle with a plug, precisely adding 50mL of 50% methanol, sealing, weighing, performing ultrasonic treatment (power 600W, frequency 40 kHz) for 30min, cooling, weighing again, supplementing the lost weight with 50% methanol, shaking, filtering, and collecting the subsequent filtrate.
2.2 Chromatographic conditions
Chromatographic condition and System applicability test
Octadecylsilane chemically bonded silica is used as a filler (column length is 250mm, inner diameter is 4.6mm, and particle diameter is 5 μm); acetonitrile-water (volume ratio is 19:81) is used as a mobile phase; the detection wavelength was 330nm. The number of theoretical plates should be not less than 3000 calculated according to acteoside peak.
Assay: respectively precisely sucking 10 μl of each of the reference solution and the sample solution, and injecting into a liquid chromatograph for measurement.
2.2.1 Determination of detection wavelength
On the basis of the above-proposed test conditions, the results of the full-band scanning of the acteoside are shown in FIG. 1.
The results showed that the optimal inspection wavelength for determining the content of acteoside in the sandalwood particles was 330 nm by analysis of the spectrogram.
2.2.2 Investigation of different mobile phases
Based on the experimental conditions set forth above, the mobile phases were acetonitrile-water (volume ratio of acetonitrile to water: 19:81), acetonitrile-0.1% formic acid (volume ratio of acetonitrile to 0.1% formic acid: 19:81), acetonitrile-0.1% phosphoric acid (volume ratio of acetonitrile to 0.1% phosphoric acid: 19:81), methanol-water (volume ratio of methanol to water: 19:81) and the results are shown in FIG. 2.
The results show that the mobile phases of acetonitrile-water, acetonitrile-0.1% formic acid and acetonitrile-0.1% phosphoric acid can well separate acteoside, while methanol-water cannot be effectively separated. However, acetonitrile-water is preferred as the mobile phase in the present invention because the presence of acidic materials in acetonitrile-0.1% formic acid, acetonitrile-0.1% phosphoric acid can cause damage to the chromatographic column.
2.3 Investigation of sample preparation methods
2.3.1 Extraction method investigation
Grinding the product, taking about 0.1 g, precisely weighing, placing into a conical flask with a plug, precisely adding 50% methanol 50 mL, sealing, weighing, ultrasonic treating (power 600W, frequency 40 kHz) or reflux extracting 30 min, cooling, weighing again, supplementing the lost weight with 50% methanol, shaking, filtering, and collecting the filtrate. The respective test solutions were separately aspirated and injected into a liquid chromatograph, and after measurement, the content of acteoside therein was calculated, and the results are shown in table 1 below.
Table 1 investigation of extraction modes
| Extraction mode | Content of acteoside (mg/g) |
| Ultrasonic wave | 10.69 |
| Reflow process | 10.70 |
The results show that the content of acteoside obtained by ultrasonic extraction and reflux extraction is not very different, and the ultrasonic extraction is selected for subsequent investigation.
2.3.2 Extraction solvent investigation
Grinding the product into fine powder, taking about 0.1g, precisely weighing, placing into conical flask with plug, precisely adding 50% methanol, 80% methanol, 50% methanol, 30% methanol and water respectively into the conical flask, sealing, weighing, ultrasonic treating (power 600W, frequency 40 kHz) for 30min, cooling, weighing, supplementing the lost weight with respective solvent, shaking, filtering, and collecting the filtrate. The respective test solutions were separately aspirated and injected into a liquid chromatograph, and after measurement, the content of acteoside therein was calculated, and the results are shown in table 2 below.
TABLE 2 extraction solvent investigation
| Extraction solvent | Content of acteoside (mg/g) |
| Methanol | 4.87 |
| 80% Methanol | 8.54 |
| 50% Methanol | 10.69 |
| 30% Methanol | 8.14 |
| 10% Methanol | 5.62 |
| Water and its preparation method | 4.68 |
The results showed that the content of acteoside was highest with 50% methanol as solvent.
2.3.3 Extraction time investigation
Grinding the product into fine powder, precisely weighing about 0.1g, placing into conical flask with plug, precisely adding 50mL of 50% methanol, sealing, weighing, ultrasonic treating (power 600W, frequency 40 kHz) for 30min, 45min, and 60min, cooling, weighing, supplementing the lost weight with 50% methanol, shaking, filtering, and collecting the filtrate. The respective test solutions were separately aspirated and injected into a liquid chromatograph, and after measurement, the content of acteoside therein was calculated, and the results are shown in table 3 below.
TABLE 3 investigation of extraction time
The result shows that the extraction time has little influence on the extraction of the acteoside, and 30min is selected as a follow-up investigation in the experiment.
2.3.4 Investigation of the addition amount of extraction solvent
Grinding the product into fine powder, precisely weighing about 0.1g, placing into conical flask with plug, precisely adding 25mL, 50mL and 100mL of 50% methanol, sealing, weighing, ultrasonic treating (power 600W, frequency 40 kHz) for 30min, cooling, weighing again, supplementing the lost weight with 50% methanol, shaking, filtering, and collecting the subsequent filtrate. The respective test solutions were separately aspirated and injected into a liquid chromatograph, and after measurement, the content of acteoside therein was calculated, and the results are shown in table 4 below.
TABLE 4 investigation of the addition amount of extraction solvent
| Solvent addition (mL) | Content of acteoside (mg/g) |
| 25 | 10.18 |
| 50 | 10.69 |
| 100 | 10.12 |
The results showed that the solvent addition was the highest at 50mL, and therefore 50mL was chosen as the final extraction solvent addition.
2.4 Methodological verification
2.4.1 Property test
Preparation of test solution: preparing a test solution of the sandalwood prescription granule according to the experimental conditions.
Preparation of a control solution: taking a proper amount of the calycosin reference substance, precisely weighing, and adding 50% methanol solution to prepare a solution containing 40 mug per 1 mL.
Preparation of negative control solution: negative control solutions lacking sandalwood particles were prepared according to the experimental conditions outlined above.
The detection result is shown in FIG. 3. The result shows that the negative control solution has no interference to the measurement of the peak to be measured, and the method has good specificity.
2.4.2 Precision test
The control solution was sampled 6 times continuously and the peak area of the acteoside was recorded. The results are shown in Table 5.
TABLE 5 precision investigation
The result shows that the instrument has good precision.
2.4.3 Repeatability test
6 Parts of sandalwood formula particles (batch number: TX-01) are precisely weighed as a test sample, a test sample solution is prepared according to the above-mentioned formulated experimental method, and the content of the acteoside in the 6 parts of test sample is calculated. The results are shown in Table 6.
Table 6 repeatability investigation
| Sequence number | Content of acteoside (mg/g) |
| 1 | 10.59 |
| 12 | 10.71 |
| 3 | 10.61 |
| 4 | 10.48 |
| 5 | 10.63 |
| 6 | 10.65 |
The result shows that the method has good repeatability.
2.4.4 Recovery
About 0.05g of a test sample (batch number: TX-01, content of acteoside 10.6 mg/g) with known content is taken, 6 parts are added, precisely weighed, acteoside reference stock solutions are respectively added precisely, preparation and measurement of test sample solution are carried out according to a planned method, and recovery rate is calculated, and the result is shown in Table 7. The calculation formula is as follows (wherein the measurement amount is the content of the acteoside measured in the sample; the content in the sample is the content of the acteoside in 0.05g of the sample; the addition amount is the content of the acteoside added to the sample before the preparation):
TABLE 7 test results of acteoside recovery
| Numbering device | Measurement result (mg) | Recovery (%) |
| 1 | 0.86551 | 100.6 |
| 2 | 0.87339 | 99.6 |
| 3 | 0.87213 | 100.3 |
| 4 | 0.86986 | 100.2 |
| 5 | 0.87012 | 100.7 |
The result shows that the method has good accuracy.
2.4.5 Linear relationship
A proper amount of acteoside is taken and placed in a 25mL volumetric flask, and is dissolved in 50% methanol to prepare a series of linear solutions containing acteoside 383.92256 mug/mL (purity 95.2%), and then diluted to the concentrations of 1.53569024 mug/mL, 7.6784512 mug/mL, 15.3569024 mug/mL, 38.392256 mug/mL, 115.176768 mug/mL and 383.92256 mug/mL respectively. Respectively, precisely sucking 10 μl, injecting into a liquid chromatograph to obtain peak area, and plotting response curve with concentration (X, μg/mL) as abscissa and peak area (Y) as ordinate, wherein the result is shown in Table 8 and FIG. 4.
TABLE 8 results of Calycosin standard curve analysis
| Sample concentration (X) | 1.53569024 | 7.6784512 | 15.3569024 | 38.392256 | 115.176768 | 383.92256 |
| Peak area (Y) | 23755 | 126518 | 255417 | 645012 | 1975828 | 6499529 |
The results show that: the linear relationship is y=16945x+345.68, and r 2 =1 when the concentration of the acteoside ranges from 1.53569024 to 383.92256 mug/mL. The concentration range is 1.53569024-383.92256 mug/mL, and the linear relation is good.
2.4.6 Intermediate precision investigation
2.4.6.1 Different instruments
Based on the experimental conditions, two parts of sandalwood formula particles (batch number: TX-01) are precisely weighed respectively to prepare test solution, the test solution is measured on an instrument 1, an instrument 2 and an instrument 3 respectively, and the content of the acteoside in the test solution is calculated. The results are shown in Table 9.
Table 9 different instrument investigation
The results show that the different instruments have good durability.
2.4.6.2 Different personnel and time investigation
Based on the experimental conditions, different persons (A, B) respectively and precisely weigh two parts of each sandalwood formula particle (batch number: TX-01) at different times (T1 and T2), prepare a test sample, measure and calculate the content of the acteoside in the test sample solution. The results are shown in Table 10.
TABLE 10 personnel and time investigation
The results show that the intermediate precision of the method is good.
2.4.7 Durability inspection
Based on the experimental conditions set forth above, the chromatographic column 1, the chromatographic column 2 and the chromatographic column 3 were examined, respectively. The results are shown in Table 11.
Table 11 column durability investigation
The results show that the method has good durability.
2.4.8 Stability investigation
Based on the experimental conditions, the same sample solution is taken, and the chromatographic peak areas of the acteoside are measured at 0h,5h,10h,15h,20h and 24h respectively. The results are shown in Table 12.
Table 12 stability investigation
| Composition of the components | 0h | 5h | 10h | 15h | 20h | 24h |
| Acteoside | 593202 | 596238 | 579999 | 581366 | 582598 | 567920 |
The results showed that the sample solution was stable for 24 hours.
2.5 Verification result of 5 batches of sandalwood formula particles
And 5 batches of samples of the product are subjected to content determination by adopting a formulated method. The results are shown in Table 13.
Table 13 results of verification of the amount of particles in the batch sandalwood formulation
| Lot number | Content of acteoside (mg/g) |
| TX-01 | 7.4 |
| TX-02 | 7.3 |
| TX-03 | 7.0 |
| TX-04 | 7.2 |
| TX-05 | 7.1 |
The result shows that the method can effectively detect the sandalwood formula particles.
Example 2
1 Laboratory apparatus and materials
Reference example 1
Sandalwood medicinal material: TX-YC-01, TX-YC-02, TX-YC-03, TX-YC-04 and TX-YC-05.
2, Establishing a method for measuring the content of medicinal materials
2.1 Sandalwood medicinal material
2.1.1 Preparation of sample solutions
Taking about 0.5g of the product (sieving with a third sieve), precisely weighing, placing in a conical bottle with a plug, precisely adding 50mL of 50% methanol solution, sealing, weighing, performing ultrasonic treatment (power 600W, frequency 40 kHz) for 30min, cooling, weighing again, supplementing the lost weight with 50% methanol solution, shaking uniformly, filtering, and taking the subsequent filtrate.
2.1.2 Preparation of control solution
Reference is made to example 1.
2.1.3 Preparation of negative solutions
Reference is made to example 1.
2.2 Chromatographic conditions
Octadecylsilane chemically bonded silica is used as a filler (column length is 250mm, inner diameter is 4.6mm, and particle diameter is 5 μm); acetonitrile-water solution (volume ratio is 19:81) is taken as a mobile phase; the detection wavelength was 330nm. The number of theoretical plates should be not less than 3000 calculated according to acteoside peak.
Assay: respectively precisely sucking 10 μl of each of the reference solution and the sample solution, and injecting into a liquid chromatograph for measurement.
2.3 Methodological verification
With reference to example 1, the method is verified by methodology, and the result shows that the method has good specificity, precision, repeatability, accuracy, durability, intermediate precision and stability, and the acteoside standard curve has good linear relation.
2.4 Verification result of 5 batches of sandalwood medicinal materials
And 5 batches of samples of the product are subjected to content determination by adopting a formulated method. As shown in table 14.
Table 14 verification of batch 5 santalum album
| Sequence number | Lot number | Acteoside content (%) | Whether or not to pass |
| 1 | TX-YC-01 | 0.31 | Qualified product |
| 2 | TX-YC-02 | 0.30 | Qualified product |
| 3 | TX-YC-03 | 0.33 | Qualified product |
| 4 | TX-YC-04 | 0.38 | Qualified product |
| 5 | TX-YC-05 | 0.70 | Qualified product |
Example 3
1 Laboratory apparatus and materials
Reference example 1
Sandalwood decoction pieces: TX-YP-01, TX-YP-02, TX-YP-03, TX-YP-04, TX-YP-05.
2 Method for measuring content of decoction pieces
2.1 Decoction pieces of Sandalwood
2.1.1 Preparation of sample solutions
Taking about 0.5g of the product (sieving with a third sieve), precisely weighing, placing in a conical bottle with a plug, precisely adding 50mL of 50% methanol solution, sealing, weighing, performing ultrasonic treatment (power 600W, frequency 40 kHz) for 30min, cooling, weighing again, supplementing the lost weight with 50% methanol solution, shaking uniformly, filtering, and taking the subsequent filtrate.
2.1.2 Preparation of control solution
Reference is made to example 1.
2.1.3 Preparation of negative solutions
Reference is made to example 1.
2.2 Chromatographic conditions
Octadecylsilane chemically bonded silica is used as a filler (column length is 250mm, inner diameter is 4.6mm, and particle diameter is 5 μm); acetonitrile-water solution (volume ratio is 19:81) is taken as a mobile phase; the detection wavelength was 330nm. The number of theoretical plates should be not less than 3000 calculated according to acteoside peak.
Assay: respectively precisely sucking 10 μl of each of the reference solution and the sample solution, and injecting into a liquid chromatograph for measurement.
2.3 Methodological verification
With reference to example 1, the method is verified by methodology, and the result shows that the method has good specificity, precision, repeatability, accuracy, durability, intermediate precision and stability, and the acteoside standard curve has good linear relation.
2.4 Verification result of 5 batches of sandalwood decoction pieces
And 5 batches of samples of the product are subjected to content determination by adopting a formulated method. As shown in table 15.
TABLE 15 verification of batch 5 Sandalwood decoction pieces
Example 4
1 Laboratory apparatus and materials
Reference example 1
Sandalwood standard decoction: TX-BT-01, TX-BT-02, TX-BT-03, TX-BT-04, TX-BT-05.
2 Standard decoction content determination method establishment
2.1 Sandalwood Standard decoction
2.1.1 Preparation of sample solutions
Taking about 0.1g of the powder, precisely weighing, placing into a conical bottle with a plug, precisely adding 50mL of 50% methanol solution, sealing, weighing, performing ultrasonic treatment (power 600W, frequency 40 kHz) for 30min, cooling, weighing again, supplementing the lost weight with 50% methanol solution, shaking, filtering, and collecting the subsequent filtrate.
2.1.2 Preparation of control solution
Reference is made to example 1.
2.1.3 Preparation of negative solutions
Reference is made to example 1.
2.2 Chromatographic conditions
Octadecylsilane chemically bonded silica is used as a filler (column length is 250mm, inner diameter is 4.6mm, and particle diameter is 5 μm); acetonitrile-water solution (volume ratio is 19:81) is taken as a mobile phase; the detection wavelength was 330nm. The number of theoretical plates should be not less than 3000 calculated according to acteoside peak.
Assay: respectively precisely sucking 10 μl of each of the reference solution and the sample solution, and injecting into a liquid chromatograph for measurement.
2.3 Methodological verification
With reference to example 1, the method is verified by methodology, and the result shows that the method has good specificity, precision, repeatability, accuracy, durability, intermediate precision and stability, and the acteoside standard curve has good linear relation.
2.4 Verification result of 5 batches of sandalwood standard decoction
And 5 batches of samples of the product are subjected to content determination by adopting a formulated method. As shown in table 12.
Table 15 verification of Sandalwood Standard decoction
It should be noted that, in the invention, chromatographic conditions and system applicability tests are carried out on the samples to be tested, namely the sandalwood medicinal materials, the sandalwood standard decoction and the sandalwood decoction pieces, and the prepared method of the samples is examined, so that the obtained conclusion is consistent with that of the samples to be tested, namely the sandalwood formula particles, and the complex samples are avoided and are not repeated.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. The method for measuring the content of the sandalwood medicinal materials, decoction pieces, standard decoction and formula particles is characterized by comprising the following steps of:
measuring the reference substance solution and the sample solution by liquid chromatography;
The reference substance in the reference substance solution is acteoside;
the conditions of the liquid chromatography are as follows: acetonitrile-water is used as a mobile phase, and the volume ratio of acetonitrile to water in the acetonitrile-water is (15-20) (80-85).
2. The method according to claim 1, wherein the volume ratio of acetonitrile to water in acetonitrile-water is (17-19): 81-83.
3. The method according to claim 1 or 2, wherein the sample solution is obtained by mixing the sample with 30 to 80 vol.% methanol and extracting the mixture.
4. The method according to claim 3, wherein the sample solution is obtained by mixing the sample with 50 vol.% methanol and extracting the mixture.
5. The method according to claim 3 or 4, wherein the mass/volume ratio of the sample solution to 30 to 80 vol.% methanol is 1 (100 to 500);
The mass volume ratio of the sample solution to 50vol% methanol is 1 (100-500);
the extraction time is not less than 30min.
6. The method according to any one of claims 1 to 5, wherein the reference solution is obtained by mixing a acteoside with 30 to 80vol% methanol and extracting;
the concentration of the acteoside in the reference substance solution is 1-384 mug/mL.
7. The method according to any one of claims 1 to 6, wherein the amounts of the control solution and the test solution to be added are each independently selected from 8 to 12. Mu.L.
8. The method according to claim 7, wherein the amount of the control solution and the sample solution added is 10. Mu.L.
9. The method according to any one of claims 1 to 8, wherein the filler of the column in the liquid chromatography is octadecylsilane chemically bonded silica;
the theoretical plate number of the chromatographic column is not less than 3000 calculated according to acteoside peak.
10. The method according to any one of claims 1 to 9, wherein the detection wavelength of the liquid chromatograph is 300 to 340nm.
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