CN113960203A - Method for detecting characteristic spectrum of tianlong formula particles - Google Patents
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Abstract
The invention relates to a method for detecting a characteristic spectrum of a tianlong formula particle, which adopts high performance liquid chromatography for analysis, adopts a chromatographic column with octadecylsilane chemically bonded silica as a filler, adopts methanol as a mobile phase A, and adopts 0.15% phosphoric acid aqueous solution as a mobile phase B for gradient elution, wherein the flow rate of the mobile phase is 0.9ml/min, the column temperature is 25-35 ℃, and the detection wavelength is 295 nm. The invention also relates to a method for establishing the contrast map of the tianlong formula particles and a method for detecting the quality of the tianlong formula particles.
Description
Technical Field
The invention belongs to the field of detection of tianlong formula particles, and particularly relates to a method for detecting a characteristic spectrum of tianlong formula particles, a method for establishing a reference spectrum of tianlong formula particles and a method for detecting the quality of tianlong formula particles.
Background
The Tianlong formula particle has better application in clinic, but a characteristic map method and a content determination method are lacked in the quality control aspect of the product, so that the construction of an analysis method of the quality standard of the Tianlong formula particle is very important.
Disclosure of Invention
In order to solve at least one technical problem, the invention provides a method for detecting a characteristic spectrum of a tianlong formula particle, a method for establishing a reference spectrum of the tianlong formula particle and a method for detecting the quality of the tianlong formula particle.
In the present invention, Gekko japonicas (Gekko et Bibron) or Gekko japonicas (Gekko et Bibron) belonging to the same genus are prepared by processing and processing dried whole Gekko japonicas belonging to Gekkonidae.
The invention provides a method for detecting a characteristic spectrum of a tianlong formula particle, which adopts high performance liquid chromatography for analysis, wherein the chromatographic conditions are as follows:
a chromatographic column: octadecylsilane chemically bonded silica gel as filler, and Shimpack Siepter C18-120, 4.6 × 250mm,5 μm as chromatographic column;
mobile phase: methanol is taken as a mobile phase A, 0.15 percent phosphoric acid aqueous solution is taken as a mobile phase B,
gradient elution: gradient elution was performed as specified in the following table, wherein% in the table below refers to volume percent,
flow rate: 0.9ml/min of the mixture is added,
column temperature: 25-35 ℃, preferably 30 ℃,
detection wavelength: 295 nm.
Particularly, the method for detecting the characteristic spectrum of the tianlong formula particles comprises the following steps:
(1) preparation of test solution
Precisely weighing the Tianlong formula granules, placing in a container with a plug, precisely adding water, weighing, ultrasonically treating, cooling, weighing again, supplementing the lost weight with water, shaking up, filtering, and taking the subsequent filtrate;
(2) chromatography analysis
And (4) measuring the test solution by using the chromatographic analysis conditions to obtain a characteristic spectrum.
In the preparation of the test solution, the mass-to-volume ratio of the tianlong formula particle to the water may be 1:20 to 1:200g/ml, preferably 1:30 to 1:100g/ml, for example, 1:50g/ml, but is not limited thereto.
Specifically, the test solution is prepared as follows: taking 0.1-1 g of the tianlong formula particles, precisely adding 5-100 ml of water, weighing, carrying out ultrasonic treatment for 10-20 minutes, cooling, weighing again, supplementing the weight loss with water, shaking up, filtering, and taking the subsequent filtrate to obtain the tianlong formula particles.
More particularly, the method for detecting the characteristic spectrum of the tianlong formula particles comprises the following steps:
(1) preparation of control solutions
Taking a proper amount of pterin-6-carboxylic acid reference substance, precisely weighing, adding ammonia water into pure water to prepare 0.028% ammonia water solution (volume percentage), and preparing into solution containing 11 mug per 1ml as reference substance solution;
(2) preparation of test solution
Taking a proper amount of the tianlong formula particles, grinding, taking about 0.5g, precisely weighing, placing in a conical flask with a plug, precisely adding 25ml of water, weighing, carrying out ultrasonic treatment (power 1130W, frequency 37kHz) for 15 minutes, cooling, weighing again, supplementing the weight loss by water, shaking up, filtering, and taking a subsequent filtrate to obtain the tianlong formula particle;
(3) chromatography analysis
And (4) measuring the reference substance solution and the test substance solution by using the chromatographic analysis conditions to obtain a characteristic spectrum.
In another aspect of the present invention, there is provided a method for establishing a control map of a tianlong formula granule, the method comprising:
preparing a plurality of sample solutions according to the method for preparing the sample solutions;
respectively detecting the plurality of sample solutions according to the method for detecting the characteristic spectrum of the tianlong formula particle to obtain a plurality of characteristic spectrums of the tianlong formula particle;
and establishing a control map of the characteristic map of the tianlong formula granules by using the obtained plurality of characteristic maps.
In the above method, the method for obtaining the control map is not particularly limited, and a conventional method in the art may be employed. For example, a reference spectrum of the tianlong formula particles can be established by introducing a plurality of obtained characteristic spectra of the tianlong formula particles into a traditional Chinese medicine chromatogram similarity evaluation system issued by the national pharmacopoeia committee. The control profile may be generated, for example, by a median method.
In particular, the control profile of the resulting Tianlong formula particles is substantially as shown in FIG. 1.
Specifically, in the control spectrum, the peak 6 is pterin-6-carboxylic acid, the peak corresponding to the peak of the reference substance of pterin-6-carboxylic acid is the S peak, the relative retention time of each characteristic peak and the S peak is calculated, and the relative retention time of each peak is:
in the method of establishing a control map of a tianlong formula granule according to the present invention, there is no particular limitation on the number of test sample solutions used to establish the control map, and a person skilled in the art can easily select an appropriate number of test sample solutions. Generally, the number of the sample solutions may be 5 or more, or 8 or more, for example, 10 or 15, and the upper limit is, for example, 30 or less, 25 or less, but not limited thereto.
The invention also provides a method for detecting the quality of the tianlong formula particles, which comprises the following steps:
(1) detecting the tianlong formula particles by using the method for detecting the characteristic spectrum of the tianlong formula particles to obtain the characteristic spectrum of the tianlong formula particles;
(2) and comparing the characteristic spectrum of the obtained Tianlong formula particle with a reference spectrum, and if the characteristic spectrum of the Tianlong formula particle contains 6 corresponding characteristic peaks in the established reference spectrum, judging that the Tianlong formula particle is qualified on the quality detection project of the characteristic spectrum.
Drawings
FIG. 1 is a control map of Gekko Swinhonis formula granules.
FIG. 2 is a chromatogram for solvent investigation of extraction of Gekko Swinhonis formula granules.
FIG. 3 is a chromatogram for examining the extraction time of Tianlong formula particles.
FIG. 4 shows different chromatographic column inspection chromatograms.
FIG. 5 is a different gradient survey chromatogram.
FIG. 6 is a chromatogram for different flow rate surveys.
FIG. 7 is a chromatogram for different column temperature examinations.
Fig. 8 is a chromatogram for different acid investigations.
Fig. 9 is a chromatogram for investigation of different acidity.
Fig. 10 is a blank solvent map.
Detailed Description
The present invention is described in detail below by way of examples. The described embodiments are illustrative only and are not to be construed as limiting the invention.
1. Instrument for measuring the position of a moving object
The instrument information used is as follows:
information of the high performance liquid chromatograph:
2 reagent
The reagent information is as follows:
3 sample and control information
The control information was as follows:
the sample information is as follows:
4. solution preparation
Preparation of test solution
Taking a proper amount of the tianlong formula granules TL-FG01, grinding, taking about 0.5g, precisely weighing, placing in a conical flask with a plug, precisely adding 25ml of water, weighing, carrying out ultrasonic treatment (the power is 1130W, the frequency is 37kHz) for 15 minutes, cooling, weighing again, complementing the weight loss by water, shaking up, filtering, and taking the subsequent filtrate to obtain the tianlong formula granule.
Preparation of control solutions
An appropriate amount of pterin-6-carboxylic acid control was weighed precisely, and ammonia water was added to pure water to prepare a 0.028% ammonia water solution (volume percentage), and the control was prepared as a solution containing 11. mu.g of the control per 1 ml.
In the following experiments, the solution formulation conditions were the same as those described herein, except for the selected conditions and the conditions specifically listed.
5. Chromatographic conditions
A chromatographic column: shimpack Siepter C18-120 column Shimadzu (column length 25cm, inner diameter 4.6mm, particle size 5 μm); methanol is taken as a mobile phase A, 0.15 percent phosphoric acid aqueous solution (volume percentage) is taken as a mobile phase B, and gradient elution is carried out according to the specification in the following table; flow rate 0.9ml per minute; the column temperature is 30 ℃; the detection wavelength was 295 nm.
In the following experiments, the chromatographic conditions were the same as here, except for the selected conditions and the conditions specifically listed.
6. Measurement method
Precisely sucking 10 μ l of each of the reference solution and the sample solution, injecting into high performance liquid chromatograph, and measuring according to specified chromatographic conditions
In the following experiments, the measurement method was the same as here, except for the selected conditions and the conditions specifically listed.
7. Examination of preparation of test sample
Considering that the dissolution conditions of the components in the sample in different extraction solvents may be different and the dissolution degree may be influenced by the time length of the ultrasonic treatment, the extraction solvent investigation and the ultrasonic treatment time investigation are performed.
7.1 examination of extraction solvent
The extraction effect of five different solvents, namely water, 10% methanol aqueous solution, 20% methanol aqueous solution, 30% methanol aqueous solution and 40% methanol aqueous solution, on the tianlong formula granules is examined, wherein the percentage is volume percentage.
Preparation of test solution
The tianlong formula particle TL-FG01 is ground, about 0.5g is taken, precisely weighed, placed in a conical flask with a plug, divided into five groups, precisely added with water, 10 percent methanol water solution, 20 percent methanol water solution, 30 percent methanol water solution and 25ml of 40 percent methanol water solution respectively, weighed, ultrasonically treated (with the power of 1130W and the frequency of 37kHz) for 15 minutes, cooled, weighed again, added with water to complement the weight loss, shaken evenly, filtered, and the subsequent filtrate is taken, thus obtaining the tianlong formula particle TL-FG 01.
The results of measurement of the obtained test solution are shown in Table 1 and FIG. 2.
TABLE 1 examination of different extraction solvents
The results show that the number of peaks of the sample does not change significantly over the range of extraction solvents examined. The methanol-water solution is easy to cause sample agglomeration and has obvious solvent effect, and water is preferably used as the extraction solvent
7.2 extraction time study
The extraction effect of the tianlong formula particles is examined after three different extraction times of 10 minutes, 15 minutes and 30 minutes.
Preparation of test solution
Grinding Tianlong formula particle TL-FG01, taking about 0.5g, precisely weighing, placing in a conical flask with a plug, dividing into three groups, precisely adding 25ml of water respectively, weighing, performing ultrasonic treatment (power 1130W, frequency 37kHz) for 10 minutes, 15 minutes and 30 minutes respectively, cooling, weighing again, supplementing the weight loss with water, shaking uniformly, filtering, and taking a subsequent filtrate to obtain the Tianlong formula particle TL-FG 01.
The results of measurement of the obtained test solution are shown in Table 2 and FIG. 3.
TABLE 2 investigation of different extraction times
The investigation result shows that the number of peaks of the sample has no obvious change in the investigated extraction time range, and the relative peak area and the relative retention time of each spectrum peak have no obvious change. Considering that the extraction time of 30 minutes is too long, the extraction time of 10 minutes is too short, and the extraction may be incomplete, the extraction time of 15 minutes is preferred.
8. Investigation of optimal chromatographic conditions
8.1 selection of detection wavelength
The pterin-6-carboxylic acid control solution is scanned in the range of 190-400nm, and the maximum absorption wavelength is 295 nm.
The test solution of the Tianlong formula particle is taken and scanned in the range of 190-400nm, the Tianlong formula particle has more peaks and better peak shape of chromatographic peak under 295nm, and therefore 295nm is taken as the optimal detection wavelength.
8.2 investigation of different chromatography columns
The influence of the columns from different manufacturers and packings (column 1: Shimpack Siepter C18-120; column 2: Shimpack GIST C18-AQ; column 3: Zishengtang C18; all 4.6 × 250mm,5 μm) on the separation effect was examined.
The results are shown in Table 3 and FIG. 4.
TABLE 3 investigation results of different chromatography columns
The investigation result shows that the chromatographic peak is seriously delayed under the condition of the chromatographic column 2; under the condition of a chromatographic column 3, a chromatographic peak is trailing; therefore, column 1 (Shimadzuk Siepter C18-120 column) is preferred.
8.3 differential gradient investigation
The characteristics of the tianlong formula granules were analyzed by the following three gradients, gradient 1, gradient 2 and gradient 3, and the results are shown in table 4 and fig. 5.
Gradient 1: 0-13 min, 1% A; 13-14 min, 1-7% A; 14-25 min, 7-15% A.
Gradient 2: 0-13 min, 1% A; 13-14 min, 1-7% A; 14-25 min, 7-20% A.
Gradient 3: 0-13 min, 1% A; 13-14 min, 1-7% A; 14-25 min, 7-10% A.
TABLE 4 examination of various gradients
The investigation result shows that when the gradient is the gradient 2, the separation degree and the tailing factor of a chromatographic peak are better, the theoretical plate number is higher, and the chromatogram is attractive, so the gradient is preferably the gradient 2.
8.4 differential flow Rate investigation
The results of the analysis of the characteristic spectrum of the Tianlong formula granules at three flow rates of 0.8ml/min, 0.9ml/min and 1.0ml/min are shown in Table 5 and FIG. 6.
TABLE 5 investigation results of different flow rates
The investigation result shows that the analysis time is prolonged under the flow rate of 0.8 ml/min; the flow rate is preferably 0.9ml/min because the theoretical plate number of the chromatographic peak is low at 1.0 ml/min.
8.5 investigation of different column temperatures
The results of analyzing the characteristic spectrum of the Tianlong formula granules at three column temperatures of 25 ℃, 30 ℃ and 35 ℃ are shown in Table 6 and FIG. 7.
TABLE 6 investigation results of different column temperatures
The investigation result shows that the theoretical plate number of the chromatographic peak is lower under the condition of 25 ℃; at 35 ℃, 6 characteristic peaks have forward extending and tailing of spectral peaks, so the temperature is preferably 30 ℃.
8.6 investigation of different acids
The characteristics of the tenglong formula granules were analyzed using 1% aqueous formic acid, 1% aqueous acetic acid and 0.15% aqueous phosphoric acid as mobile phases B, respectively, and the results are shown in table 7 and fig. 8.
Table 7 examination of different acids
The results of the investigation show that when mobile phase B additive is 1% acetic acid, chromatographic peaks 1 and 2 combine to form an inclusion peak; when the mobile phase B additive is 1% formic acid, the chromatographic peak 4 does not reach baseline separation; when the mobile phase B is 0.15% phosphoric acid, 6 chromatographic peaks are excellent, and therefore, 0.15% phosphoric acid is preferred as the acid.
8.7 investigation of differential acidity
The characteristics of the tenglong formula granules were analyzed using 0.17% phosphoric acid aqueous solution, 0.13% phosphoric acid aqueous solution, and 0.15% phosphoric acid aqueous solution as mobile phases B, respectively, and the results are shown in table 8 and fig. 9.
TABLE 8 examination of different acidity
As a result of examination, it was found that when mobile phase B was a 0.15% phosphoric acid aqueous solution, 6 chromatographic peak shapes were excellent, and therefore, a 0.15% phosphoric acid aqueous solution was preferable.
8.8 Final defined chromatographic conditions
The chromatographic conditions finally determined were as follows:
a chromatographic column: shimpack Siepter C18-120 column Shimadzu (column length 25cm, inner diameter 4.6mm, particle size 5 μm);
mobile phase: methanol is taken as a mobile phase A, and 0.15% phosphoric acid aqueous solution is taken as a mobile phase B;
gradient conditions: gradient elution was performed as specified in the table below;
flow rate: 0.9ml per minute;
column temperature: 30 ℃;
detection wavelength: 295 nm.
9. Methodology investigation
9.1 specificity
Taking a pure water sample, directly injecting sample according to the finally determined chromatographic conditions, and recording a 25-minute chromatogram as shown in figure 10. The results show that the system has no residue and interference.
9.2 precision
Taking the sample solution, continuously injecting sample 6 needles under the finally determined chromatographic conditions, and recording the chromatogram.
The relative retention time of each characteristic peak and the S peak and the RSD% value of the relative peak area were calculated using peak 6 (peak of pterin-6-carboxylic acid) as the S peak, and the results are shown in Table 9.
TABLE 9 Instrument precision investigation
The investigation result shows that the relative retention time RSD% and the relative peak area RSD% of each characteristic peak in the 6-needle sample solution are both less than 2.00%, and the instrument precision of the method is good.
9.3 repeatability
Taking the tianlong formula particle TL-FG01 to prepare 6 parts of test solution, analyzing under the finally determined chromatographic conditions, and recording a chromatogram.
The relative retention time of each characteristic peak and the S peak and the RSD value of the relative peak area were calculated using peak No. 6 (peak of pterin-6-carboxylic acid) as the S peak, and the results are shown in Table 10.
TABLE 10 repeatability test
The investigation result shows that the relative retention time RSD% and the relative peak area RSD% of each characteristic peak in the 6-needle parallel sample are both less than 2.00%, which indicates that the method for detecting the characteristic spectrum of the tianlong formula particles has good repeatability.
9.4 intermediate precision
Taking the Tianlong formula particle TL-FG01, preparing 3 parallel sample solutions at different dates and by different persons, respectively, measuring under the finally determined chromatographic conditions in different instruments (Waters e 269503, Waters e 269502, Waters e 269504), and recording chromatograms.
The relative retention time of each characteristic peak to the S peak and the RSD value of the relative peak area were calculated using pterin-6-carboxylic acid (peak No. 6) as the S peak, and the results are shown in Table 11.
Experiment 1: day one, person one, Waters e 269503
Experiment 2: day two, person two, Waters e 269502
Experiment 3: third day, third person, Waters e 269504
TABLE 11 intermediate precision investigation
The investigation result shows that the relative retention time RSD% is less than 2%, and the relative peak area RSD% is less than 10%, which shows that the method for detecting the characteristic spectrum of the tianlong formula particles has good intermediate precision.
9.5 stability
The sample solution is taken and placed for 0h, 2h, 4h, 6h, 8h, 10h, 12h, 18h and 24h at room temperature respectively, and then sample injection analysis is carried out under the finally determined chromatographic conditions, and the results are shown in Table 12.
TABLE 12 sample stability Studies
The result shows that the relative peak area RSD% and the relative retention time RSD% of 6 characteristic peaks of the test solution are less than 1% within 24 hours, and the stability is good.
10. Establishment of control map
Respectively preparing test solution by using 10 batches of skyron formula particles with sample batch numbers of TL-FG01, TL-FG02, TL-FG03, TL-FG04, TL-FG05, TL-FG06, TL-FG07, TL-FG08, TL-FG09 and TL-FG10 produced by Shanghai Wanshi medicine industry Co., Ltd, and performing sample injection analysis under the finally determined chromatographic conditions to obtain 10 characteristic chromatograms.
Fitting the 10 obtained characteristic chromatograms by using a national pharmacopoeia committee 'traditional Chinese medicine chromatogram fingerprint similarity evaluation system' (2012 edition) to generate a control chromatogram of the tianlong formula granules, which is shown in figure 1.
FIG. 1 is a control graph of a Gekko Swinhonis formula granule, wherein peak 6 is pterin-6-carboxylic acid, the peak corresponding to the reference peak of pterin-6-carboxylic acid is the S peak, and the relative retention time of each characteristic peak and the S peak is calculated as: 0.269 (peak 1), 0.340 (peak 2), 0.462 (peak 3), 0.600 (peak 4), 0.827 (peak 5), 1.000 (peak 6).
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that 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 (10)
1. A method for detecting a characteristic spectrum of Tianlong formula particles is characterized in that the method adopts high performance liquid chromatography for analysis, and the chromatographic conditions are as follows:
a chromatographic column: octadecylsilane chemically bonded silica gel as filler, and Shimpack Siepter C18-120, 4.6 × 250mm,5 μm as chromatographic column;
mobile phase: methanol is taken as a mobile phase A, 0.15 percent phosphoric acid aqueous solution is taken as a mobile phase B,
gradient elution: gradient elution was performed as specified in the following table, wherein% in the table below refers to volume percent,
flow rate: 0.9ml/min of the mixture is added,
column temperature: 25-35 ℃, preferably 30 ℃,
detection wavelength: 295 nm.
2. The method of claim 1, comprising the steps of:
(1) preparation of test solution
Precisely weighing the Tianlong formula granules, placing in a container with a plug, precisely adding water, weighing, ultrasonically treating, cooling, weighing again, supplementing the lost weight with water, shaking up, filtering, and taking the subsequent filtrate;
(2) chromatography analysis
The test sample solution is subjected to measurement using the chromatographic conditions described in claim 1 to obtain a characteristic map.
3. The method according to claim 2, wherein the test solution is prepared such that the weight/volume ratio of the tianlong formula particles to the water is 1:20 to 1:200g/ml, preferably 1:30 to 1:100 g/ml.
4. The method of claim 2, wherein the sample solution is prepared by: taking 0.1-1 g of the tianlong formula particles, precisely adding 5-100 ml of water, weighing, carrying out ultrasonic treatment for 10-20 minutes, cooling, weighing again, supplementing the weight loss with water, shaking up, filtering, and taking the subsequent filtrate to obtain the tianlong formula particles.
5. The method of claim 1, comprising the steps of:
(1) preparation of control solutions
Taking a proper amount of pterin-6-carboxylic acid reference substance, precisely weighing, adding ammonia water into pure water to prepare an ammonia water solution with the volume percentage of 0.028%, and preparing the solution into a solution with the volume percentage of 11 mu g/ml to serve as a reference substance solution;
(2) preparation of test solution
Taking a proper amount of the tianlong formula particles, grinding, taking 0.5g, precisely weighing, placing in a conical flask with a plug, precisely adding 25ml of water, weighing, carrying out ultrasonic treatment at the power of 1130W and the frequency of 37kHz for 15 minutes, cooling, weighing again, supplementing the weight loss by water, shaking up, filtering, and taking the subsequent filtrate to obtain the tianlong formula particle;
(3) chromatography analysis
The control solution and the test solution are subjected to measurement using the chromatographic conditions as set forth in claim 1 to obtain characteristic maps.
6. A method of establishing a control profile for a tianlong formula granule, the method comprising:
preparing a plurality of test solution using the method of preparing a test solution according to any one of claims 2 to 5;
detecting the plurality of test solution solutions respectively by using the chromatographic conditions as described in claim 1 to obtain a plurality of characteristic maps of the tianlong formula particles;
and establishing a control map of the characteristic map of the tianlong formula granules by using the obtained plurality of characteristic maps.
7. The method of claim 6, wherein the control profile of the Gekko Swinhonis formula is substantially as shown in figure 1.
8. The method according to claim 7, wherein in the control profile, peak 6 is pterin-6-carboxylic acid, the relative retention time of each characteristic peak to the S peak is calculated using the peak corresponding to the pterin-6-carboxylic acid reference peak as the S peak, and the relative retention time of each peak is:
9. the method of claim 6, wherein the number of the sample solutions is 5 or more.
10. A method for detecting the quality of Tianlong formula granules comprises the following steps:
(1) testing a tianlong formula using a method according to any one of claims 1 to 5 to obtain a characteristic profile of the tianlong formula;
(2) and comparing the characteristic spectrum of the obtained Tianlong formula particle with a reference spectrum, and if the characteristic spectrum of the Tianlong formula particle contains 6 corresponding characteristic peaks in the established reference spectrum, judging that the Tianlong formula particle is qualified on the quality detection project of the characteristic spectrum.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115144522A (en) * | 2022-06-02 | 2022-10-04 | 江阴天江药业有限公司 | Control method for comprehensively controlling quality of gecko formula granules |
| CN115144522B (en) * | 2022-06-02 | 2023-09-22 | 江阴天江药业有限公司 | Control method for comprehensively controlling quality of gecko formula particles |
| CN115326985A (en) * | 2022-08-30 | 2022-11-11 | 北京康仁堂药业有限公司 | Centipede formula particle characteristic spectrum and construction method and application thereof |
| CN115326985B (en) * | 2022-08-30 | 2023-06-02 | 北京康仁堂药业有限公司 | Centipede formula granule characteristic spectrum and construction method and application thereof |
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