CN115343389A - HPLC detection method for liquiritigenin in Changdu caragana - Google Patents
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Abstract
The invention discloses an HPLC detection method of liquiritigenin in Changda caragana, which comprises the following steps: 1) Preparation of a control solution: dissolving glycyrrhizin reference substance in methanol to obtain reference substance solution; 2) Preparing a test solution: taking a sample to be detected, adding methanol for extraction, filtering an extracting solution, and taking a filtrate as a test solution; 3) Respectively sucking the reference solution and the test solution and injecting into a high performance liquid chromatograph; the chromatographic conditions were as follows: a chromatographic column: octadecylsilane chemically bonded silica is used as a filling agent; mobile phase: volume ratio 68:32 of 0.1% formic acid water and methanol. The invention realizes the complete separation of the important composition liquiritigenin in the Changda caragana through a specific sample pretreatment method and chromatographic conditions, finally establishes a method for measuring the content of the liquiritigenin in the Changda caragana, can meet the accurate, sensitive, simple, convenient and rapid measuring principle, and perfects the quality control method of the Changda caragana.
Description
Technical Field
The invention relates to an HPLC detection method of liquiritigenin in Changda caragana.
Background
Tibetan caragana (Lignum Caraganae), also known as "Zuoxiang", is a red woody plant of various caragana plants of Leguminosae (Leguminosae) produced in Qinghai-Tibet plateau, and is an important Tibetan medicine for breaking blood and removing blood stasis. Caragana coprinus (caragana (pall.) poir.) and caragana changdu (c. Caragana microphylla has the effects of promoting blood circulation and removing blood stasis, and is commonly used for treating diseases such as hypertension, hyperemia, irregular menstruation and the like. Modern pharmaceutical chemistry research shows that the main chemical components of the caragana tibetana are flavonoid compounds represented by isoflavone and pterocarpin. At present, few research reports about qualitative and quantitative evaluation and quality evaluation of caragana tibetana are reported, and the research is mainly focused on the research of flavonoid components in caragana microphylla.
Wei Yongsheng, and the like, a method for measuring the content of flavonoid compounds in Tibetan medicine Jinjia caragana is disclosed in China pharmaceutical journal, 2015, 40 (1), but researches report that HPLC fingerprints of Jinjia caragana and Changdu caragana are greatly different, the substance components in the two are different, and the important component liquiritigenin in Changdu caragana cannot be detected by the disclosed method.
Disclosure of Invention
In order to solve the problems, the invention provides an HPLC detection method of liquiritigenin in Caragana lacustris, which comprises the following steps:
1) Preparation of a reference solution: dissolving glycyrrhizin reference substance in methanol to obtain reference substance solution;
2) Preparing a test solution: taking a sample to be detected, adding methanol for extraction, filtering an extracting solution, and taking a filtrate as a test solution;
3) Respectively sucking the reference solution and the test solution, and injecting into a high performance liquid chromatograph; the chromatographic conditions were as follows:
a chromatographic column: octadecylsilane chemically bonded silica is used as a filling agent; mobile phase: volume ratio 68:32 of 0.1% formic acid water and methanol.
Further, the mass-to-volume ratio of the reference substance in the step 1) to the methanol solution is 20-100 μ g:1ml.
Further, the volume ratio of the sample to be detected in the step 2) to methanol is 1ml:50 to 150ml.
Further, the extraction in the step 2) is ultrasonic extraction for 60min.
Further, step 3) the chromatographic conditions are that the column: kromasil C18 column, 4.6mm x 250mm,5 μm, column temperature 20-40 deg.C, sample amount 10-50 μ L, flow rate 0.8-1.2 ml/min, detection wavelength: 230 or 278nm.
Further, the column temperature is 40 ℃, the sample injection amount is 10 μ L, the flow rate is 1ml/min, and the detection wavelength: 278nm.
Further, the content of the liquiritigenin in the sample to be detected is calculated by peak area according to an external standard method.
Further, the sample to be tested is a powder of Caragana lacustris.
The HPLC detection method of liquiritigenin in the Changda caragana of the invention realizes the complete separation of important composition liquiritigenin in the Changda caragana through a specific sample pretreatment method and chromatographic conditions, finally establishes a method for measuring the content of liquiritigenin in the Changda caragana, can meet the accurate, sensitive, simple, convenient and rapid measurement principle, and perfects the quality control method of the Changda caragana.
Obviously, many modifications, substitutions, and variations are possible in light of the above teachings of the invention, without departing from the basic technical spirit of the invention, as defined by the following claims.
The present invention will be described in further detail with reference to the following examples. This should not be understood as limiting the scope of the above-described subject matter of the present invention to the following examples. All the technologies realized based on the above contents of the present invention belong to the scope of the present invention.
Drawings
Figure 1 shows HPLC chart of Changda caragana with different feed-liquid ratios ((1) feed-liquid ratio 1
FIG. 2 Total wavelength scan of glycyrrhizin
FIG. 3 HPLC charts of different proportions of 0.1% aqueous formic acid (A) methanol (B) ((1) 0.1% aqueous formic acid (A) -32% methanol (B) (2) 0.1% aqueous formic acid (A) -35% methanol (B) (3) 0.1% aqueous formic acid (A) -38% methanol (B))
FIG. 4 Changda caragana HPLC chart with different flow rates ((1) 0.8ml/min flow rate (2) 1ml/min flow rate (3)
FIG. 5 HPLC chart of Changda caragana with different column temperatures ((1); column temperature of 20 deg.C (2); column temperature of 30 deg.C (3); column temperature of 40 deg.C)
FIG. 6 high performance liquid chromatogram of control, changdu caragana sample and negative control
FIG. 7 Liquiritigenin standard curve
Detailed Description
The reagents, reagents and equipment used in the embodiment of the present invention are known products and obtained by purchasing commercially available products.
EXAMPLE 1 detection of Liquiritigenin in Caragana changdu according to the present invention
1) Preparation of control solutions
Weighing glycyrrhizin reference substance, precisely weighing, adding methanol to obtain solution containing 51 μ g of glycyrrhizin per 1ml, and diluting with methanol to obtain reference substance solutions with series concentrations;
2) Preparation of test solution
Taking 1g of Changdu caragana powder, accurately weighing, placing in a conical flask with a plug, accurately adding 50ml of methanol, sealing the plug, weighing, ultrasonically extracting for 60min, cooling, weighing again, complementing the weight loss by methanol, shaking uniformly, filtering through a 0.45 mu l microporous filter membrane, and taking the subsequent filtrate to obtain a test solution;
3) Precisely sucking 10 μ l of the reference solution and the sample solution, respectively, injecting into a liquid chromatograph, and recording chromatogram. The chromatographic conditions were as follows:
a chromatographic column: kromasil C18 column (4.6 mm. Times.250mm, 5 μm); mobile phase 0.1% aqueous formic acid (a) -methanol (B) =68:32, a first step of removing the first layer; column temperature: at 40 ℃; detection wavelength: 278nm; flow rate: 1mL/min -1 。
4) Respectively drawing standard curves by taking the mass concentration (X) of the liquiritigenin in the reference solution as an abscissa and taking the peak area (Y) as an ordinate, and calculating the content of the liquiritigenin in the Caragana changdi according to the standard curves.
The beneficial effects of the present invention are illustrated by the following experimental examples:
test example 1
1. Laboratory instruments and materials
1.1 instruments
The main experimental instruments are shown in Table 1
TABLE 1 Main Experimental Equipment
1.2 reagents
The main experimental reagents are shown in Table 2.
TABLE 2 Main test reagents
1.3 samples
The experiment totally collects 25 batches of medicinal materials, and the serial numbers are from 1 to 25. All the drug samples were identified as red wood heartwood of Caragana changdu (Caragana changduensis y.x. Liou) of Caragana of the genus leguminosae by professor of Jianguihua traditional Chinese medicine university, and the original plants were rechecked by professor of waiwas of traditional Chinese medicine institute of Sichuan province. The information collected on the samples of Changda caragana is shown in Table 3.
TABLE 3 sample Collection information Table
2. Examination of method for preparing test solution
In the known literature, the Tibetan medicine of caragana contains flavonoids as the most main chemical components, and liquiritigenin also belongs to flavonoids compounds. No separation and detection method of the liquiritigenin in the Changda caragana is provided by reference of related documents, so that an HPLC detection method of the liquiritigenin of the Changda caragana is constructed by investigating an extraction solvent, an extraction method and a material-liquid ratio of a Tibetan medicine, the content of the liquiritigenin of the Changda caragana to be tested.
2.1 examination of extraction solvent
The solvent extraction study comprises 50% methanol, ethanol, 50% ethanol and methanol. Respectively taking 1g of Changdu caragana powder, precisely weighing, respectively placing in a conical flask with a plug, precisely adding 50% methanol, ethanol, 50% ethanol and methanol, sealing the plug, weighing, treating at 40 ℃ with ultrasound (power 100W and frequency 45 kHz) for 60min, weighing again, complementing the weight loss with corresponding solvent, shaking up, filtering, taking subsequent filtrate, and filtering with a microporous filter membrane to obtain the final product. The content was measured under the chromatographic conditions under the term "3.5", and the results are shown in Table 4.
TABLE 4 examination of extraction solvent
As can be seen from the table, methanol was selected as the extraction solvent because of the highest content of glycyrrhizin extracted with methanol.
2.2 examination of extraction methods
The experiment researches five different extraction methods and extraction time of 30min, 60min and 90min of ultrasound, 30min and 60min of reflux. Weighing 1g of caragana changdu powder, precisely weighing, placing in a conical flask with a plug, precisely adding 50ml of methanol, sealing, weighing, respectively treating with ultrasound (power 100W, frequency 45 kHz) for 30min, 60min and 90min, refluxing for 30min and 60min, cooling, weighing again, supplementing the weight loss with methanol, shaking, filtering, and filtering the filtrate with 0.45 μm microporous membrane. The content was measured under the chromatographic conditions under the term "3.5", and the results are shown in Table 5.
TABLE 5 method of extraction investigation results
As can be seen from the table, the extraction effect of the liquiritigenin extracted by ultrasonic and reflux for 60min is close. Along with the prolonging of the ultrasonic extraction time, the extraction effect of the liquiritigenin is slightly increased. Therefore, ultrasonic extraction is selected for 60min.
2.3 investigation of the ratio of liquid to feed
The experiment investigated four different feed-to-liquid ratios of the sample powder of changda caragana to the methanol extraction solvent of 1. Weighing 0.5g of four parts of Changda caragana powder, precisely weighing, respectively placing in 50ml conical bottles with stoppers, marking as No. 1, no. 2, no. 3 and No. 4, precisely adding 10ml of methanol into No. 1, precisely adding 20ml of methanol into No. 2, precisely adding 25ml of methanol into No. 3, precisely adding 50ml of methanol into No. 4, sealing, weighing, treating for 60min by ultrasonic (power 100W and frequency 45 kHz) at 40 ℃, weighing again, complementing the weight loss by using corresponding solvent, shaking up, filtering, taking the subsequent filtrate, and filtering with a microporous filter membrane to obtain the final product. The content was measured according to the chromatographic conditions under "3.5" and the results are shown in Table 6 and FIG. 1.
TABLE 6 investigation results of the ratio of liquid to feed
As can be seen from the graph, the contents of the latter two liquid-to-solid ratios are high, and considering the material cost, 1.
2.4 determination of the preparation method of the test solution
According to the investigation result of the 3 factors, the preparation method of the test sample is determined as follows: precisely weighing 1g of Changda caragana powder, placing in a conical flask with a plug, precisely adding 50ml of methanol, sealing, weighing, ultrasonically extracting for 60min, cooling, weighing again, supplementing the lost weight with methanol, shaking, filtering, and collecting the subsequent filtrate.
3. Investigation of chromatographic conditions
At present, no report on the determination of the liquiritigenin content in the Changda caragana is seen, so that the detection wavelength, the mobile phase, the flow velocity and the column temperature of the determination of the liquiritigenin content in the Changda caragana are screened and investigated.
3.1 selection of detection wavelength
Taking liquiritigenin reference substance 10.61mg, precisely weighing, dissolving in methanol, transferring into 25ml volumetric flask, adding methanol to desired volume, and making into solution containing liquiritigenin 51 μ g per 1ml methanol.
A Kromasil C18 (250 mm multiplied by 4.6mm,5 mu m) chromatographic column is selected, the detection wavelength is examined under the conditions of the same mobile phase, flow velocity and column temperature, and a detector is arranged to perform full-wavelength scanning at the wavelength of 190-400 nm. The results are shown in FIG. 2.
The result shows that the liquiritigenin reference substance has maximum absorption peaks at 230nm and 278nm, which is consistent with the absorption peaks of liquiritigenin reported by related documents, so the detection wavelength is selected to be 278nm.
3.2 selection of the Mobile phase
A Kromasil C18 (250 mm multiplied by 4.6mm,5 mu m) chromatographic column is selected, and under the conditions of the same flow rate, column temperature and detection wavelength, the experiment respectively investigates a plurality of mobile phases and different proportions: (1) 0.1% aqueous formic acid (A) -acetonitrile (B) (18% B,20% B,22% B,23% B,24% B,25% B); (2) 0.1% aqueous formic acid (A) -methanol (B) (22% B,25% B,30% B,32% B,35% B,38% B); (3) water (a) -32% methanol (B). The same batch of samples was tested under different mobile phase systems. Partial results are shown in FIG. 3.
The results showed that the ratio of (a) -methanol (B) =68:32, the base line is smooth, the separation degree of each absorption peak in the chromatogram is good, and the retention time is appropriate, so that the volume ratio of 68:32 of 0.1% aqueous formic acid (A) -methanol (B) were used as the mobile phase for the determination of the content.
3.3 selection of flow Rate
A Kromasil C18 (250 mm multiplied by 4.6mm,5 mu m) chromatographic column is selected, and under the conditions of the same mobile phase, column temperature and detection wavelength, 3 flow rates are respectively examined at this time: (1) 0.8ml/min, (2) 1.0ml/min, (3) 1.2ml/min. The same batch of samples was tested at different flow rates. The results are shown in FIG. 4.
The results show that the base lines of the 3 flow rates are stable, the separation degree of each peak is good, the column pressure is ideal when the flow rate is 1ml/min, and the retention time is appropriate. Therefore, the flow rate is preferably 1 ml/min.
3.4 selection of column temperature
According to the literature, a Kromasil C18 (250 mm multiplied by 4.6mm,5 μm) chromatographic column is selected, and under the conditions of the same flow rate, column temperature and detection wavelength, 3 column temperatures are respectively considered in this time: (1) the same batch of samples was examined at different column temperatures, 20 deg.C, (2), 30 deg.C and (3) 40 deg.C. The results are shown in FIG. 5.
The result shows that no peak appears in 70min under the condition of 20 ℃, and the separation degree of the liquiritigenin and adjacent peaks is good and the time is relatively fast under 40 ℃, so 40 ℃ is taken as the optimal column temperature.
3.5 determination of chromatographic conditions
By examining the above 4 conditions, the chromatographic conditions for content measurement of Changda caragana using liquiritigenin as an index were determined. The following: a chromatographic column: kromasil C18 (4.6 mm. Times.250mm, 5 μm); mobile phase: 0.1% aqueous formic acid (a) -32% methanol (B); detection wavelength: 278nm; flow rate: 1ml/min; column temperature: 40 ℃; sample introduction amount: 10 μ l.
4. Methodology investigation
Methodology investigation is mainly an assessment of established analytical methods, including system applicability experiments, linear relationship investigation, precision, stability, repeatability, sample recovery, durability, etc. The experiment inspects the items and evaluates the established method for measuring the content of the liquiritigenin in the Changda caragana.
4.1 System suitability test
Taking the reference solution, the sample solution and the negative reference solution (methanol), respectively performing sample injection determination under the chromatographic condition of "2.5", and recording chromatogram, as shown in FIG. 6. The separation degree between the liquiritigenin and the adjacent peak is more than 1.5, the theoretical plate number is not less than 3000 according to the liquiritigenin, and negative control shows no interference.
4.2 Linear relationship examination
Preparation of control solution Glycyrrhrizae radix control 10.61mg is precisely weighed, diluted 50 times with methanol, and then 4 times to obtain a solution with a concentration of 212.2 μ g/ml -1 、53.05μg·ml -1 The storage liquid (1) and the storage liquid (2). Precisely measuring the stock solutions (2, 0.5ml, 1ml, 2ml and 5 ml), placing 3.75 and 5ml of the stock solutions (1) in 10ml volumetric flasks, adding methanol solution to constant volume to obtain reference solutions with series concentrations. The sample is injected and measured according to the chromatographic condition under the item of '2.5', and the mass concentration (mu g/ml) is measured -1 ) Linear regression was performed with the abscissa (X) and the peak area (mAU min) the ordinate (Y), and the results are shown in table 6 and fig. 7.
4.3 precision test
The control solution 5 under the term "3.4.2" was taken and continuously measured for 6 times under the chromatographic conditions under the term "2.5", and the peak area was recorded as shown in Table 7. As a result, the RSD value of the liquiritigenin peak area is less than 3.00 percent, which indicates that the precision of the instrument is good.
4.4 stability test
Taking the sample solution, injecting samples at different times of 0, 4, 8, 12, 16 and 24h under the chromatographic condition of '2.5', measuring, and recording peak areas, which is shown in Table 10. The result shows that the RSD value of the liquiritigenin peak area is less than 3.00 percent, which shows that the test solution has good stability within 24 hours.
4.5 repeatability test
Taking 6 parts of the same batch of samples of the Changda caragana, preparing a test solution under the item '3.3', measuring under the chromatographic condition under the item '2.5', recording peak areas, and calculating the content of the liquiritigenin, which is shown in a table 10. The results show that the RSD values of the liquiritigenin content are all less than 3.00 percent, and the method has good repeatability.
TABLE 10 results of the repeatability tests
4.6 sample recovery test
0.5g of the same sample of the same lot of the chamelameles changdu is taken, 6 parts are taken in parallel and precisely weighed, 5ml of reference substance stock solution (1) is respectively added, a test solution is prepared under the item of 3.3, the chromatographic condition is measured under the item of 2.5, the peak area is recorded, and the recovery rate of the liquiritigenin is calculated and shown in Table 12. The result shows that the sample adding recovery rate of the liquiritigenin is 95-110%, which shows that the method has good accuracy.
TABLE 11 sample recovery test results
4.7 durability examination
Taking the same batch of Caragana changdi samples, preparing a test solution under the item ' 3.3 ', and respectively inspecting 3 different types of chromatographic columns { (1) { (WelchultimateLP-C) by using an instrument (1) under the chromatographic condition under the item ' 2.5 18 (250mm×4.6mm，5μm)、②WatersXTERRARRP18(250mm×4.6mm，5μm)、③KromasilC 18 (250 mm. Times.4.6 mm,5 μm) }; investigation of 3 different models of HPLC { (1) } (1) Using column (3)Instruments (agilent corporation); (2) PE-A10 high performance liquid chromatograph (Perkin Elmer); (3) the influence of an Agilent1100 high performance liquid chromatograph (Agilent corporation) on the content determination of liquiritigenin. The results are shown in Table 13, and the RSD values of the liquiritigenin content detected by different chromatographic columns and different instruments are all less than 3.00 percent, which shows that the durability is good.
TABLE 12 durability test results (different columns)
5. Determination of sample content
5.1 moisture determination
According to the operation regulation of a drying method in pharmacopoeia of the people's republic of China, 2-5g of a test sample is taken, precisely weighed, dried at 100-105 ℃ for 5 hours, moved to a dryer, cooled for 30min, precisely weighed, dried at the temperature for 1h, cooled, weighed and weighed until the difference between two successive weighing is not more than 5 mg. The water content was calculated and is shown in Table 13.
5.2 sample content determination
A sample of the Changdu caragana is taken, a test solution is prepared under the item '3.4', sample injection measurement is carried out under the chromatographic condition under the item '2.5', the peak area of the chromatographic peak of the liquiritigenin is recorded, and the content is calculated, which is shown in Table 13.
TABLE 13 sample content and moisture measurements
6. Conclusion and discussion
The content measurement is an important component in the quality standard of the traditional Chinese medicinal materials. On the basis of reference documents, the method for measuring the content of the Changda caragana is systematically investigated and constructed, HPLC chromatographic conditions and a preparation method of a test solution are determined, and the method for measuring the content of the Changda caragana is finally established. Can meet the accurate, sensitive, simple and rapid determination principle.
Chromatographic conditions are as follows: a Kromasil C18 (4.6 mm. Times.250mm, 5 μm) column was used; by volume ratio 68:32 of 0.1% formic acid aqueous solution (A) -methanol (B) were subjected to isocratic elution at a detection wavelength of 278nm at a flow rate of 1ml/min at a column temperature of 40 ℃.
Preparation of control solution: taking appropriate amount of glycyrrhizin reference substance, precisely weighing, adding methanol solution to obtain solution containing 51 μ g per 1ml
Preparation of a test solution: precisely weighing 1g of Changdu caragana powder, placing in a conical flask with a plug, precisely adding 50ml of methanol, sealing the plug, weighing, ultrasonically extracting for 60min, cooling, weighing again, supplementing the lost weight with methanol, shaking up, filtering through a 0.45 mu l microporous filter membrane, and taking the subsequent filtrate to obtain the test solution.
The measuring method comprises the following steps: precisely sucking 10 μ l of each of the reference solution and the sample solution, injecting into liquid chromatography, and measuring.
The methodology investigation examines the system applicability, linear relationship, precision, stability, repeatability, sample recovery rate and durability. The standard curve shows good linear relation, the relative deviation of precision, stability and repeatability is less than 3%, the sample recovery rate is 95-110%, and the accuracy is good. The results are all in a reliable range, which indicates that the content determination method of the Changdu caragana obtained by the experiment is feasible.
In conclusion, the invention realizes the complete separation of the important composition liquiritigenin in the Changdu caragana through a specific sample pretreatment method and chromatographic conditions, finally establishes a method for measuring the content of the liquiritigenin in the Changdu caragana, can meet the accurate, sensitive, simple, convenient and rapid measuring principle, and perfects the quality control method of the Changdu caragana.
Claims (8)
1. An HPLC detection method of liquiritigenin in championss changdu is characterized by comprising the following steps: it comprises the following steps:
1) Preparation of a reference solution: dissolving glycyrrhizin reference substance in methanol to obtain reference substance solution;
2) Preparing a test solution: taking a sample to be detected, adding methanol for extraction, filtering an extracting solution, and taking a filtrate as a test solution;
3) Respectively sucking the reference solution and the test solution and injecting into a high performance liquid chromatograph; the chromatographic conditions were as follows:
a chromatographic column: octadecylsilane chemically bonded silica is used as a filling agent; mobile phase: volume ratio 68:32 of 0.1% formic acid water and methanol.
2. An HPLC assay method according to claim 1, characterized in that: the mass volume ratio of the reference substance to the methanol solution in the step 1) is 20-100 mug: 1ml.
3. An HPLC assay method according to claim 1, characterized in that: step 2) the volume ratio of the sample to be detected to methanol is 1ml:50 to 150ml.
4. An HPLC assay method according to claim 1, characterized in that: the extraction in the step 2) is ultrasonic extraction for 60min.
5. The HPLC detection method according to claim 1, wherein: step 3) chromatographic conditions in the chromatographic column: kromasil C18 column, 4.6mm x 250mm,5 μm, column temperature 20-40 deg.C, sample amount 10-50 μ L, flow rate 0.8-1.2 ml/min, detection wavelength: 230 or 278nm.
6. An HPLC detection method according to claim 5, characterized in that: the column temperature is 40 ℃, the sample injection amount is 10 mu L, the flow rate is 1ml/min, and the detection wavelength is as follows: 278nm.
7. An HPLC detection method according to any one of claims 1 to 6, characterized in that: the content of the liquiritigenin in the sample to be detected is calculated by peak area according to an external standard method.
8. The HPLC detection method of claim 7, wherein: the sample to be detected is powder of Changdu caragana.
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