CN113533598B - High performance liquid chromatography analysis method for content of scutellaria baicalensis in infantile lung heat cough and asthma granules - Google Patents
High performance liquid chromatography analysis method for content of scutellaria baicalensis in infantile lung heat cough and asthma granules Download PDFInfo
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- CN113533598B CN113533598B CN202110874249.5A CN202110874249A CN113533598B CN 113533598 B CN113533598 B CN 113533598B CN 202110874249 A CN202110874249 A CN 202110874249A CN 113533598 B CN113533598 B CN 113533598B
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
The invention provides a high performance liquid chromatography analysis method for content of scutellaria baicalensis in particles for treating infantile lung heat cough and asthma, which comprises the following steps: (1) preparing a test solution: taking a particle test sample for infantile lung heat cough and asthma, taking a tri-n-octylphosphine oxide ethanol solution as a solvent, sealing, carrying out ultrasonic treatment, cooling to room temperature, and continuously using the tri-n-octylphosphine oxide ethanol solution for constant volume to prepare a test sample solution; (2) preparing a reference substance solution: precisely weighing baicalin reference substance, and preparing reference substance solution with ethanol solution of tri-n-octylphosphine oxide as solvent; (3) chromatographic conditions: respectively taking the reference solution and the sample solution, injecting into a high performance chromatograph for determination, and performing gradient elution by using 2, 4-dimethyl-3-pentanol as a mobile phase A, tributyl phosphate as a mobile phase B and ethanol as a mobile phase C. The method can effectively detect under the condition of near room temperature, not only can prolong the service life of the chromatographic column, but also has reliable detection result.
Description
Technical Field
The invention relates to the field of pediatric drug detection, in particular to a high performance liquid chromatography analysis method for content of scutellaria baicalensis in pediatric lung heat cough and asthma granules.
Background
The infantile lung-heat cough and asthma particle is a compound preparation of eleven traditional Chinese medicines, has the functions of clearing heat and detoxicating, freeing lung and relieving cough, and reducing phlegm and asthma, and is mainly used for cold, bronchitis, asthmatic bronchitis and bronchopneumonia caused by phlegm-heat obstructing lung. The scutellaria baicalensis has the main functions of clearing heat and drying dampness, purging fire and removing toxicity, stopping bleeding and preventing miscarriage and the like, has a long history of medication, and is one of the traditional Chinese medicine varieties commonly used in Chinese medicine clinical practice. Baicalin is one of the effective components of scutellaria baicalensis, and modern pharmacological research proves that the baicalin has broad-spectrum antibacterial, antiviral and antipyretic effects and has definite anti-inflammatory effect. Therefore, baicalin as one of the active ingredients of the product can be used as a basis for measuring the content of scutellaria in the particles for treating the infantile lung heat cough and asthma. Referring to the existing methods, such as the method for detecting the content of baicalin in scutellaria baicalensis and paeonia lactiflora, the column temperature is 40 ℃, the long-term use of the chromatographic column is not facilitated, the stability of the chromatographic column is also influenced, the service life of the chromatographic column is shortened, and the detection effect is not ideal.
Disclosure of Invention
In view of this, the invention provides a high performance liquid chromatography analysis method for the content of scutellaria baicalensis in the infantile lung heat cough and asthma granules, and solves the problems.
The technical scheme of the invention is realized as follows:
a high performance liquid chromatography analysis method for content of scutellaria baicalensis in infantile lung heat cough and asthma granules comprises the following steps:
(1) Preparing a test solution: taking a particle test sample for infantile lung heat cough and asthma, taking a tri-n-octylphosphine oxide ethanol solution as a solvent, sealing, carrying out ultrasonic treatment, cooling to room temperature, and continuously using the tri-n-octylphosphine oxide ethanol solution for constant volume to prepare a test sample solution;
(2) Preparing a reference substance solution: precisely weighing baicalin reference substance, and preparing reference substance solution with ethanol solution of tri-n-octylphosphine oxide as solvent;
(3) Chromatographic conditions are as follows: respectively taking the reference solution and the sample solution, injecting into a high performance chromatograph for determination, and performing gradient elution by using 2, 4-dimethyl-3-pentanol as a mobile phase A, tributyl phosphate as a mobile phase B and ethanol as a mobile phase C.
Further, the ethanol solution of the tri-n-octylphosphine oxide is prepared by mixing the tri-n-octylphosphine oxide and ethanol according to a mass ratio of 5-10: 90-95.
Further, the ultrasonic treatment time is 2-4min, the ultrasonic power is 100-120W, the ultrasonic frequency is 20-25kHz, the preferable ultrasonic treatment time is 3min, the ultrasonic power is 110W, and the ultrasonic frequency is 23kHz.
Further, the elution procedure was:
| mobile phase A (v/v) | Mobile phase B | Mobile phase C | |
| 0-8.00 | 63％ | 12％ | 25％ |
| 8.01-15.00 | 55％ | 35％ | 10％ |
| 15.01-30.00 | 35％ | 55％ | 10％ |
| 30.01-40.00 | 12％ | 63％ | 25％ |
Further, INERTSUSTAIN C18 chromatographic column with length of 150mm, inner diameter of 3.0mm, and filler particle size of 3 μm is used.
Furthermore, the column temperature is 23-28 ℃, the flow rate is 0.8-1.2ml/min, and the detection wavelength is 272-282 nm. Preferably, the column temperature is 25 ℃, the flow rate is 1.0ml/min, and the detection wavelength is 277nm.
Compared with the prior art, the invention has the beneficial effects that:
by adopting the high performance liquid chromatography analysis method, the flow combined gradient elution is preferably selected, the column temperature is effectively reduced, the detection can be effectively carried out under the condition of near room temperature, the service life of the chromatographic column can be prolonged, the peak shape is good, the separation from other adjacent peaks is good, the content of the baicalin in the infantile lung heat cough and asthma particles can be well detected, and the linear relation, the repeatability, the precision, the quantitative limit and the like of the detection method are good. And moreover, the optimized compound solvent is adopted, so that the ultrasonic power and time are reduced, the solvent loss is reduced, and the detection stability is improved.
Drawings
FIG. 1 is a photograph of an HPLC chromatogram of a test solution in example 1 of the present invention;
FIG. 2 is a HPLC chromatogram of a control solution of example 1 of the present invention.
Detailed Description
In order that the technical contents of the invention may be better understood, specific examples are provided below to further illustrate the invention.
The experimental methods used in the examples of the present invention are all conventional methods unless otherwise specified.
The materials, reagents and the like used in the examples of the present invention can be obtained commercially without specific description.
Example 1
Taking a sample of the infantile lung-heat cough and asthma particle, and detecting according to the following steps:
(1) Preparing a solvent: the method is characterized in that the method comprises the following steps of (1) preparing a mixture of tri-n-octyl phosphine oxide and ethanol according to a mass ratio of 5:95 mixing to obtain a tri-n-octyl phosphine oxide ethanol solution, namely a solvent;
(2) Preparing a test solution: taking about 0.4g of the infant lung-heat cough and asthma particle sample, finely grinding and weighing, placing the sample in a 50ml volumetric flask, adding the tri-n-octylphosphine oxide ethanol solution (solvent) obtained in the step (1), sealing, carrying out ultrasonic treatment for 3min, wherein the ultrasonic power is 110W, the ultrasonic frequency is 23kHz, cooling to room temperature, continuously using the tri-n-octylphosphine oxide ethanol solution obtained in the step (1) to fix the volume to prepare a sample solution, taking a subsequent filtrate, filtering the subsequent filtrate by using a 0.45 mu m microporous filter membrane, and taking the subsequent filtrate as the sample solution;
(3) Preparing a reference substance solution: precisely weighing baicalin reference substance, dissolving with ethanol solution of tri-n-octylphosphine oxide in step (1) as solvent, diluting to constant volume, making into solution containing baicalin about 60 μ g per lml to obtain reference substance solution, filtering with 0.45 μm microporous membrane, and collecting filtrate.
(4) Chromatographic conditions are as follows: respectively taking the reference solution and the sample solution, injecting into a high performance chromatograph for determination, and injecting into a sample volume of 10 μ l. Taking 2, 4-dimethyl-3-pentanol as a mobile phase A, tributyl phosphate as a mobile phase B and ethanol as a mobile phase C, and carrying out gradient elution, wherein the elution procedure is as follows:
| mobile phase A (v/v) | Mobile phase B | Mobile phase C | |
| 0-8.00 | 63％ | 12％ | 25％ |
| 8.01-15.00 | 55％ | 35％ | 10％ |
| 15.01-30.00 | 35％ | 55％ | 10％ |
| 30.01-40.00 | 12％ | 63％ | 25％ |
Detection conditions are as follows: adopting INERTSSUSTAIN C18 chromatographic column with length of 150mm, inner diameter of 3.0mm, filler particle size of 3 μm,
the column temperature was 25 c,
the flow rate was 1.0ml/min,
the detection wavelength was 277nm.
As shown in FIG. 1, a photograph of an HPLC chromatogram of the test solution (sample) of example 1 is shown.
As shown in fig. 2, a HPLC profile photograph of the control solution of example 1.
The baicalin peak in the test sample chromatogram has good shape, and is well separated from other adjacent peaks.
Example 2
Using the chromatographic conditions of example 1, on the basis of example 1, a solvent consisting of tri-n-octylphosphine oxide and ethanol in a mass ratio of 10:90 by mixing.
Example 3
The control solution and the test solution prepared in example 1 were used, and the column temperature in the chromatographic conditions was adjusted to 23 ℃ based on example 1.
Example 4
The control solution and the test solution prepared in example 1 were used, and the column temperature in the chromatographic conditions was adjusted to 28 ℃ based on example 1.
Example 5
The control solution and the test solution prepared in example 1 were used, and the flow rate under the chromatographic conditions was adjusted to 0.8ml/min based on example 1.
Example 6
The control solution and the test solution prepared in example 1 were used, and the flow rate under the chromatographic conditions was adjusted to 1.2ml/min based on example 1.
Example 7
The control solution and the test solution prepared in example 1 were used, and the detection wavelength in the chromatographic conditions was adjusted to 272nm based on example 1.
Example 8
The control solution and the test solution prepared in example 1 were used to adjust the detection wavelength in the chromatographic conditions to 282nm based on example 1.
Comparative example 1
On the basis of example 1, no gradient elution was used, using a volume ratio of 47:53:0.2 of methanol-water-phosphoric acid is used as a mobile phase. The results showed that baicalin peak shape was not good and tailing factor was more than 1.5.
Comparative example 2
On the basis of example 1, no gradient elution was used, using a volume ratio of 1:1:1, 2, 4-dimethyl-3-pentanol, tributyl phosphate and ethanol as mobile phases. The results showed that baicalin had a poor peak shape with a tailing factor of less than 1.5.
Test examples
The chromatographic conditions of example 1 were examined methodically. The results are as follows:
2.1 System suitability test
Test and control solutions were prepared as in example 1.
The experimental results show that the number of theoretical plates is higher than 4600 (calculated as baicalin peak). And the system applicability requirement is met (the number of theoretical plates is higher than 2500).
2.2 Linear relationship test
Taking 10.45mg (the content is 94.0%) of baicalin reference substance, precisely weighing, placing in a 50ml measuring flask, adding 5wt% of tri-n-octylphosphine oxide ethanol solution for dissolving and diluting to scale, and shaking up. And respectively precisely measuring 3 ml, 4 ml, 5 ml, 6 ml and 7ml, putting into a 10ml measuring flask, adding a 5wt% tri-n-octylphosphine oxide ethanol solution for diluting to a scale, and shaking up. The measurement was carried out under the chromatographic conditions of example 1.
The experimental results are as follows: the linear equation is: y =37218x-60709, R =0.9999, the result shows that the baicalin reference substance is 58.464 ∞In the concentration range of 137.415 mu g/ml, the linear relation (R) with the peak area is good 2 ＝0.9999)。
2.3 precision
2.3.1 precision of sample injection: the baicalin reference solution (prepared according to example 1) is measured by different analysts in the same laboratory at intervals of one day by using two different liquid phases (the first phase is double-pump-automatic sample injection and the second phase is single-pump-manual sample injection), the average value of the peak area is calculated, and the precision of the measurement by the analysts by using different equipment is inspected. Precisely measuring 10 μ l of reference solution, injecting into liquid chromatograph, recording chromatogram, and repeating the measurement for 6 times. The results show that the precision of the instrument is good.
2.3.2 intermediate precision: test solutions were prepared as in example 1. The content of the extract is measured by two liquid chromatographs in the same laboratory at intervals of one day by different analysts, and the average content (mg/g) is calculated by taking 6 samples each time. The content of all samples was 10.02mg/g on average, and the RSD was 1.05%. The results show that the intermediate precision is good.
2.3.3 repeatability testing of samples
Test and control solutions were prepared according to the examples. The measurement was carried out under the chromatographic conditions of example 1. The average value was 9.74mg/g, and the RSD was 0.78%. The results show good reproducibility.
2.4 limit of quantitation
With a signal-to-noise ratio of 10: taking the sample concentration at 1 hour as the limit of the product, precisely weighing 10.13mg (94.0%) of baicalin control, adding 5wt% ethanol solution of tri-n-octylphosphine oxide, gradually diluting, and filtering. Debugging a chromatograph, sampling 10 mu l of samples with different concentrations after the base line is stable, and recording a chromatogram; from the chromatogram, it is known that: when the concentration of the test solution is 0.0096 mu g/ml, the signal-to-noise ratio of the main peak is 10:1, the minimum quantitative limit of this product is 0.096ng (0.0096. Mu.g/ml. Times.10. Mu.l). The quantitative limit concentration sample is continuously injected for 6 times, the RSD% of the main peak retention time is 0.11%, the RSD% of the peak area is 1.45%, and the requirements that the RSD% of the main peak retention time is not more than 2.0% and the RSD% of the main peak area is not more than 5.0% are met.
2.5 sample application recovery test
Taking the product, preparing three concentrations according to 80%, 100% and l20%, respectively, preparing three samples at each concentration, adding the product reference substance in equal proportion into 9 samples, preparing 9 sample solutions according to the above method, and performing sample loading and recovery test. The above solution was taken and measured under the chromatography conditions of example 1. Precisely measuring 10 μ l, injecting into a liquid chromatograph, and recording chromatogram. And taking another reference substance solution, measuring by the same method, and calculating by peak area according to an external standard method to obtain the final product.
The result shows that the recovery rate is 99.01-100.12% and the RSD is 0.35-1.34% in the concentration range of 80-120%, and the requirements of 95-105% and RSD <5% are met. The experimental result shows that the product has good recovery rate test.
2.6 solution stability test
A sample solution was prepared in accordance with the method of example 1, and the subsequent filtrate was allowed to stand at room temperature for 12 hours, and then injected after 0, 2,4, 6, 8, 10, and 12 hours, respectively, and the peak area thereof was measured to examine the stability of the solution.
The test result shows that the peak area RSD of each time point is 0.13%, and the product is basically stable after being placed at room temperature for 12 hours.
2.7 determination of baicalin content in this product
The baicalin content of three samples of the product with the same specification (4 g per bag) was measured according to the measurement method of example 1, and the results are as follows.
Children lung heat cough and asthma particle baicalin content determination result
| Batch number | 150501 | 150502 | 150503 |
| Baicalin content mg/bag | 40.21 | 40.25 | 39.98 |
In addition, the content of scutellaria baicalensis in the infantile lung heat cough and asthma granules is detected by adopting the same batch of test products according to the examples 2-8. The results show that the retention time of the baical skullcap root peak, the tailing factor (less than 1.1) and the separation degree (more than 1.9) of each example meet the requirements.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (8)
1. A high performance liquid chromatography analysis method for content of scutellaria baicalensis in particles for treating infantile lung heat cough and asthma is characterized by comprising the following steps:
(1) Preparing a test solution: taking a particle test sample for infantile lung heat cough and asthma, taking a tri-n-octylphosphine oxide ethanol solution as a solvent, sealing, carrying out ultrasonic treatment, cooling to room temperature, and continuously using the tri-n-octylphosphine oxide ethanol solution for constant volume to prepare a test sample solution;
(2) Preparing a reference substance solution: precisely weighing baicalin reference substance, and preparing reference substance solution with ethanol solution of tri-n-octylphosphine oxide as solvent;
(3) Chromatographic conditions are as follows: respectively taking a reference substance solution and a sample solution, injecting the reference substance solution and the sample solution into a high-efficiency chromatograph for determination, taking 2, 4-dimethyl-3-pentanol as a mobile phase A, taking tributyl phosphate as a mobile phase B, taking ethanol as a mobile phase C, and carrying out gradient elution, wherein the elution procedure is as follows:
；
An INERTSUSTAIN C18 chromatographic column with a length of 150mm, an inner diameter of 3.0mm and a filler particle size of 3 μm is adopted.
2. The HPLC analysis method for Scutellariae content in infantile lung heat cough and asthma granule according to claim 1, wherein the ethanol solution of trioctylphosphine oxide is prepared from trioctylphosphine oxide and ethanol at a mass ratio of 5-10: 90-95.
3. The HPLC analysis method for Scutellariae content in infantile lung-heat cough and asthma granule according to claim 1 or 2, wherein the ultrasonic treatment time is 2-4min, the ultrasonic power is 100-120W, and the ultrasonic frequency is 20-25kHz.
4. The HPLC analysis method of Scutellariae content in the infantile lung heat cough and asthma granule as claimed in claim 1, wherein the column temperature is 23-28 deg.C.
5. The HPLC analysis method for Scutellariae content of infantile lung heat cough and asthma granule as claimed in claim 1, wherein the flow rate is 0.8-1.2ml/min.
6. The HPLC analysis method for Scutellariae content in infantile lung-heat cough and asthma granule according to claim 1, wherein the detection wavelength is 272-282 nm.
7. The HPLC analysis method for Scutellariae content in infantile lung-heat cough and asthma granule according to claim 1, wherein in step (1), the ultrasonic treatment time is 3min, the ultrasonic power is 110W, and the ultrasonic frequency is 23kHz.
8. The HPLC analysis method for Scutellariae content in infantile lung-heat cough and asthma granule as claimed in claim 1, wherein the column temperature is 25 ℃.
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| US5032216A (en) * | 1989-10-20 | 1991-07-16 | E. I. Du Pont De Nemours And Company | Non-photographic method for patterning organic polymer films |
| WO1996002528A1 (en) * | 1994-07-14 | 1996-02-01 | Tsumura & Co. | Method of separating and recovering flavone compound having glycoside structure and flavone compound not having glycoside structure |
| CN1207301C (en) * | 2003-05-25 | 2005-06-22 | 韩桂茹 | Process of extracting baicalin from scutellaria baicalensis |
| BR112013011874A2 (en) * | 2010-11-11 | 2019-09-24 | Akron Molecules Gmbh | compounds and methods for treating pain |
| CN105395616A (en) * | 2013-12-02 | 2016-03-16 | 李兴惠 | Injection for clearing heat, eliminating phlegm and removing toxicity |
| CN105866267B (en) * | 2016-03-29 | 2018-08-31 | 福建中烟工业有限责任公司 | The extraction of residual solvent, detection method and kit and purposes in packaging material |
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