CN107894473B - HPLC method for detecting aconitic acid content in pinellia ternata - Google Patents
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Abstract
The invention provides application of a method for detecting the aconitic acid content in pinellia ternata quality detection, and in addition, the invention provides an HPLC method for detecting the aconitic acid content in pinellia ternata. The method can accurately and effectively detect the cis-aconitic acid content and the trans-aconitic acid content in the pinellia ternata, and lays a foundation for improving the quality control level of the pinellia ternata and promoting the development and utilization of medicinal materials.
Description
Technical Field
The invention relates to an HPLC method for detecting aconitic acid content in pinellia ternata.
Background
The rhizoma Pinelliae is dried tuber of rhizoma Pinelliae Pinellia ternata (Thunb.) Breit of Pinellia of Araceae. Has effects of eliminating dampness and phlegm, lowering adverse qi and relieving vomit, and relieving oppression and resolving hard mass. Can be used for treating damp phlegm and cold phlegm, cough, asthma, excessive phlegm, phlegm retention, dizziness, palpitation, wind phlegm, vertigo, phlegm syncope, headache, emesis, regurgitation, feeling of fullness in chest and epigastrium, and globus hystericus; it is indicated for abscess with phlegm nodule.
Pinellia ternata is complex in component and contains various organic acids, alkaloids, proteins and the like, wherein the organic acids are important pharmacodynamic ingredients for exerting curative effects. At present, the succinic acid content is often used as an evaluation standard for the quality of pinellia ternate, for example, the total organic acid content is calculated and determined by adopting a potentiometric titration method in the Chinese pharmacopoeia 2015 edition, and the quality of pinellia ternate is controlled. The method has the advantages of complex operation, high possibility of being influenced by other organic acids and operation conditions, large error, inaccurate measurement and nonideal quality control of the pinellia ternata. There are also a few reports on measuring the contents of organic acids such as oxalic acid, malic acid, citric acid, succinic acid and the like in pinellia ternata, but the evaluation indexes are still not complete.
Therefore, in order to control the quality of pinellia ternata comprehensively, it is necessary to further search for evaluation indexes and measurement methods for measuring organic acids in pinellia ternata.
Disclosure of Invention
The invention aims to provide a novel method for detecting the quality of semi-summer.
The inventor firstly discovers in research that pinellia ternate contains 2 new organic acids of cis-aconitic acid and trans-aconitic acid, and carries out separation and content measurement on the organic acids.
The invention provides application of a method for detecting the content of aconitic acid in pinellia ternata quality detection.
Wherein the aconitic acid is cis-form and/or trans-form aconitic acid.
The invention provides a method for detecting the content of aconitic acid in pinellia ternata, which comprises the following steps:
a. preparing a test solution:
ultrasonic extracting rhizoma Pinelliae powder, centrifuging, collecting supernatant, adding phosphoric acid, mixing, extracting with ethyl acetate, evaporating, and dissolving with mobile phase to obtain sample solution;
b. preparation of control solutions:
dissolving cis-aconitic acid and/or trans-aconitic acid reference substance in water to obtain reference substance solution;
c. respectively injecting the test solution and the reference solution into a high performance liquid chromatograph for detection, wherein the chromatographic conditions are as follows:
a chromatographic column: a C18 chromatography column;
mobile phase: the mobile phase is methanol (or acetonitrile) -0.1% phosphoric acid solution (3-10: 97-90);
detection wavelength: 210 nm;
d. and calculating the content of cis-aconitic acid and/or trans-aconitic acid in the pinellia ternata according to the detection result.
Wherein, in the step a, the solvent for ultrasonic extraction is water or 80% methanol.
Wherein the amount of water is 20-50mL per 1g of pinellia ternate powder; preferably, 50mL of water is used per 1g of pinellia tuber powder.
Wherein, in the step a, 0.1ml of phosphoric acid is used for every 25ml of supernatant; and/or the number of extractions with ethyl acetate is 5.
Wherein the ultrasonic extraction time is 15-120 minutes; preferably, the extraction time is 60 minutes.
In step c, the specification of the chromatographic column is as follows: the inner diameter is 4.6mm, the length is 250mm, and the grain diameter of the filler is 5 mu m; a preferred column model is the Inertsil ODS-3C18 column.
Wherein, in the step c, the mobile phase is methanol-0.1% phosphoric acid solution (3:97), acetonitrile-0.1% phosphoric acid solution (3:97) or methanol-0.1% phosphoric acid solution (10: 90).
Wherein the column temperature of the chromatographic condition is 25-35 ℃; the flow rate is 0.5-0.8 mL/min;
preferably, the column temperature is 35 ℃; the flow rate was 0.8 mL/min.
The inventor successfully establishes an HPLC method for measuring the cis-aconitic acid content and the trans-aconitic acid content in the pinellia ternate by screening an extraction method and chromatographic conditions, the method is accurate, reliable, simple, convenient and quick, lays a foundation for analyzing the organic acid content of the pinellia ternate and improving the overall quality control of the pinellia ternate, is beneficial to the development and utilization of pinellia ternate medicinal materials, and has good application prospects.
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 blank sample HPLC chromatogram.
FIG. 2 is a HPLC chart of a control; wherein 1 is cis-aconitic acid and 2 is trans-aconitic acid.
FIG. 3 HPLC chromatogram of pinellia ternata sample (example 1 method); wherein 1 is cis-aconitic acid and 2 is trans-aconitic acid.
FIG. 4 HPLC chromatogram of pinellia ternata sample (example 2 method); wherein 1 is cis-aconitic acid and 2 is trans-aconitic acid.
FIG. 5 HPLC chromatogram of pinellia ternata sample (example 3 method); wherein 1 is cis-aconitic acid and 2 is trans-aconitic acid.
FIG. 6 HPLC chromatogram of pinellia ternata sample (example 4 method); wherein 1 is cis-aconitic acid and 2 is trans-aconitic acid.
Detailed Description
The following examples are further illustrative, but the present invention is not limited to these examples.
Example 1 HPLC method of the invention
The method comprises the following steps:
1. preparing a test solution:
taking about 1g of pinellia ternate sample powder (screened by a sieve of four numbers), precisely weighing, placing the sample powder in a 150mL conical flask, adding 50mL of water, weighing, ultrasonically treating for 60 minutes, cooling, weighing again, complementing the weight loss by water, centrifuging, precisely weighing 25mL of supernate, adding 0.1mL of phosphoric acid, shaking up, extracting for 5 times by ethyl acetate, 20mL each time, combining ethyl acetate, evaporating to dryness, adding methanol (or acetonitrile) -0.1% phosphoric acid solution (3:97) into residues, dissolving, fixing the volume to 5mL, filtering, and taking the subsequent filtrate to obtain the pinellia ternate.
2. Preparation of control solutions
Precisely weighing control substances cis-aconitic acid and trans-aconitic acid, dissolving in water, and shaking.
Preparing a blank sample: the blank sample was prepared as follows: taking a 150mL conical flask, adding 50mL of water, weighing, carrying out ultrasonic treatment for 60 minutes, cooling, weighing again, supplementing the lost weight with water, centrifuging, precisely weighing 25mL of clear solution, adding 0.1mL of phosphoric acid, shaking up, extracting with ethyl acetate for 5 times, 20mL each time, combining ethyl acetate, evaporating to dryness, adding methanol-0.1% phosphoric acid solution (3:97) into residues for dissolving, fixing the volume to 5mL, filtering, and taking the subsequent filtrate to obtain the product.
3. Respectively injecting the test solution and the reference solution into a high performance liquid chromatograph for detection, wherein the chromatographic conditions are as follows:
an Agilent 1200 high performance liquid chromatograph (DAD detector), Inertsil ODS-3C18(4.6 × 250mm, 5 μm) chromatographic column, methanol-0.1% phosphoric acid solution (3:97) as mobile phase, flow rate of 0.8mL/min, detection wavelength of 210nm, and column temperature of 35 deg.C.
4. And calculating the contents of cis-aconitic acid and trans-aconitic acid in the pinellia ternata according to the detection result.
The results are shown in FIGS. 1 to 3.
Therefore, the method can effectively measure the cis-aconitic acid and the trans-aconitic acid in the pinellia ternata.
Example 2 HPLC method of the invention
The method comprises the following steps:
1. preparing a test solution: the same as in example 1.
2. Preparation of control solutions: the same as in example 1.
3. Respectively injecting the test solution and the reference solution into a high performance liquid chromatograph for detection, wherein the chromatographic conditions are as follows:
an Agilent 1200 high performance liquid chromatograph (DAD detector), Inertsil ODS-3C18(4.6 × 250mm, 5 μm) chromatographic column, acetonitrile-0.1% phosphoric acid solution (3:97) as mobile phase, flow rate of 0.8mL/min, detection wavelength of 210nm, and column temperature of 35 deg.C.
4. And calculating the contents of cis-aconitic acid and trans-aconitic acid in the pinellia ternata according to the detection result.
The results are shown in FIG. 4.
Therefore, the method can effectively measure the cis-aconitic acid and the trans-aconitic acid in the pinellia ternata.
Example 3 HPLC method of the invention
The method comprises the following steps:
1. preparing a test solution: the same as in example 1.
2. Preparation of control solutions: the same as in example 1.
3. Respectively injecting the test solution and the reference solution into a high performance liquid chromatograph for detection, wherein the chromatographic conditions are as follows:
an Agilent 1200 high performance liquid chromatograph (DAD detector), Inertsil ODS-3C18(4.6 × 250mm, 5 μm) chromatographic column, methanol-0.1% phosphoric acid solution (3:97) as mobile phase, flow rate of 0.5mL/min, detection wavelength of 210nm, and column temperature of 25 deg.C.
4. And calculating the contents of cis-aconitic acid and trans-aconitic acid in the pinellia ternata according to the detection result.
The results are shown in FIG. 5.
Therefore, the method can effectively measure the cis-aconitic acid and the trans-aconitic acid in the pinellia ternata.
Example 4 HPLC method of the invention
The method comprises the following steps:
1. preparing a test solution: the same as in example 1.
2. Preparation of control solutions: the same as in example 1.
3. Respectively injecting the test solution and the reference solution into a high performance liquid chromatograph for detection, wherein the chromatographic conditions are as follows:
an Agilent 1200 high performance liquid chromatograph (DAD detector), Inertsil ODS-3C18(4.6 × 250mm, 5 μm) chromatographic column, methanol-0.1% phosphoric acid solution (10:90) as mobile phase, flow rate of 0.5mL/min, detection wavelength of 210nm, and column temperature of 25 deg.C.
4. And calculating the contents of cis-aconitic acid and trans-aconitic acid in the pinellia ternata according to the detection result.
The results are shown in FIG. 6.
Therefore, the method can effectively measure the cis-aconitic acid and the trans-aconitic acid in the pinellia ternata.
The following test examples specifically illustrate the advantageous effects of the present invention:
test example 1 Process parameter screening of the method of the present invention
First, experimental material
1. Medicinal material source
The pinellia ternate is prepared from pinellia ternate test field in Penian county, Nangaoshi, Sichuan province by peeling and drying.
2. Instruments, reagents
An Agilent 1200 high performance liquid chromatograph (DAD detector), Inertsil ODS-3C18(4.6 × 250mm, 5 μm) chromatographic column, electronic balance (Sadolis scientific instruments Co., Ltd.), water bath (Beijing Zhongxing Wei instruments Co., Ltd.), drying box, rotary evaporator (Heldolph, Germany), circulating water type multipurpose vacuum pump, HY-4A digital display speed regulation multipurpose oscillator, and centrifuge (Beckmancoulter, USA).
Cis-aconitic acid and trans-aconitic acid are purchased from Chinese family and have purity higher than 98%.
Methanol, acetonitrile, ethyl acetate and phosphoric acid are used as chromatographic purities, water is ultrapure water, and the rest is analytical purities.
Second, screening by the method of the present invention
Preparation of control solutions
Respectively and precisely weighing 10.20mg and 11.46mg of cis-aconitic acid, trans-aconitic acid, water dissolving, and shaking.
(II) preparation of test solution
The inventor inspects the extraction method, the extraction solvent, the extraction time and the dosage of the extraction solvent of the test sample, and concretely comprises the following steps:
1. examination of extraction method
Taking 1g of pinellia ternate sample powder (screened by a sieve IV), precisely weighing, adding 50mL of water, weighing, carrying out ultrasonic treatment or heating reflux for 60 minutes, cooling, weighing again, complementing the weight loss by water, centrifuging, precisely weighing 25mL of supernatant, adding 0.1mL of phosphoric acid, shaking up, extracting for 5 times by using ethyl acetate, 20mL each time, combining the ethyl acetate, evaporating to dryness, adding methanol (or acetonitrile) -0.1% phosphoric acid solution (3:97) into residues, dissolving, fixing the volume to 5mL, and filtering to obtain a subsequent filtrate.
Taking 20 μ l of test solution, injecting into high performance liquid chromatograph, and calculating the content of 2 kinds of aconitic acid with mixed solution of cis-aconitic acid and trans-aconitic acid as reference substance.
The chromatographic conditions were that Inertsil ODS-3C18(4.6 × 250mm, 5 μm) was used as a chromatographic column, a methanol-0.1% phosphoric acid solution (3:97) was used as a mobile phase, the flow rate was 0.8mL/min, the detection wavelength was 210nm, and the column temperature was 35 ℃.
The results are shown in Table 1.
TABLE 1 results of different extraction methods
As can be seen from table 1, 2 kinds of aconitic acid can be extracted only by the ultrasonic extraction method, 2 kinds of aconitic acid cannot be extracted by the reflux extraction method, and starch in pinellia ternata is easily gelatinized by heating and refluxing extraction at high temperature during the extraction process, which is not favorable for subsequent centrifugation and component extraction.
Therefore, an ultrasonic extraction method is selected to prepare a sample to be detected.
2. Examination of extraction solvent
Different solvents were selected and the effect of both water and 80% methanol extraction solvents was examined according to the ultrasonic extraction method described above. The results are shown in Table 2.
TABLE 2 results of different extraction solvent treatments
As can be seen from Table 2, aconitic acid was extracted with all of the 2 solvents, and the water extraction effect was the best. Therefore, water is chosen as the extraction solvent.
2. Investigation of extraction time
Ultrasonic treating with water as extraction solvent for 15, 30, 60, and 120min, and observing extraction time. The results are shown in Table 3.
TABLE 3 processing results for different extraction times
As can be seen from Table 3, 2 types of aconitic acid can be effectively extracted when the ultrasonic time is 30-120min, and the extraction time is selected to be 60min in order to ensure the sufficient extraction of different samples.
4. Investigation of extraction solvent dosage
Taking about 1g of sample powder (passing through a sieve of No. four), precisely weighing, adding 20mL, 30mL, 40 mL and 50mL of water, weighing, ultrasonically treating for 60min, cooling, weighing again, complementing the weight loss with water, centrifuging, precisely weighing supernatant, adding 0.1mL of phosphoric acid, shaking up, extracting for 5 times with ethyl acetate, 20mL each time, combining ethyl acetate, evaporating to dryness, dissolving the residue with methanol (or acetonitrile) -0.1% phosphoric acid solution (3:97), fixing the volume to 5mL, filtering, and taking the subsequent filtrate to obtain the product. The extraction time was examined.
Taking 20 μ l of test solution, injecting into high performance liquid chromatograph, and calculating the content of 2 kinds of aconitic acid with mixed solution of cis-aconitic acid and trans-aconitic acid as reference substance.
The chromatographic conditions were that Inertsil ODS-3C18(4.6 × 250mm, 5 μm) was used as a column, a methanol-0.1% phosphoric acid solution (3:97) was used as a mobile phase, the flow rate was 0.8mL/min, the detection wavelength was 210nm, and the column temperature was 35 ℃ and the results are shown in Table 4.
TABLE 4 investigation of different amounts of extraction solvent
As shown in Table 4, 2 kinds of aconitic acid were extracted efficiently with 20-50ml of water, and 50ml is preferable because the pinellia tuber starch content is high and the pinellia tuber powder is not easily dispersed when the liquid volume is small.
Therefore, the finally determined optimal preparation method of the test solution comprises the following steps: sampling 1g of powder (passing through a sieve of four numbers), precisely weighing, placing in a conical flask with a plug, adding 50mL of water, weighing, ultrasonically treating for 60 minutes, cooling, weighing again, complementing the weight loss with water, centrifuging, precisely weighing 25mL of supernatant, adding 0.1mL of phosphoric acid, shaking up, extracting for 5 times with ethyl acetate, 20mL each time, combining ethyl acetate, evaporating to dryness, dissolving the residue with methanol (or acetonitrile) -0.1% phosphoric acid solution (3:97), fixing the volume to 5mL, filtering, and taking the subsequent filtrate to obtain the product.
In conclusion, the inventor discovers in research that the pinellia ternate contains 2 new organic acids of cis-aconitic acid and trans-aconitic acid, and successfully establishes an HPLC (high performance liquid chromatography) method for measuring the cis-aconitic acid content and the trans-aconitic acid content in the pinellia ternate by screening an extraction method and chromatographic conditions.
Claims (13)
1. Application of a method for detecting the content of aconitic acid in pinellia ternata in the quality detection of pinellia ternata.
2. Use according to claim 1, characterized in that: the aconitic acid is cis-form and/or trans-form aconitic acid.
3. A method for detecting the content of aconitic acid in pinellia ternata is characterized by comprising the following steps: the method comprises the following steps:
a. preparing a test solution:
ultrasonic extracting rhizoma Pinelliae powder, centrifuging, collecting supernatant, adding phosphoric acid, mixing, extracting with ethyl acetate, evaporating, and dissolving with mobile phase to obtain sample solution;
b. preparation of control solutions:
dissolving cis-aconitic acid and/or trans-aconitic acid reference substance in water to obtain reference substance solution;
c. respectively injecting the test solution and the reference solution into a high performance liquid chromatograph for detection, wherein the chromatographic conditions are as follows:
a chromatographic column: a C18 chromatography column;
mobile phase: the mobile phase is 3:97 methanol-0.1% phosphoric acid solution, volume ratio 3:97 acetonitrile-0.1% phosphoric acid solution or volume ratio 10: 90% methanol-0.1% phosphoric acid solution;
detection wavelength: 210 nm;
d. and calculating the content of cis-aconitic acid and/or trans-aconitic acid in the pinellia ternata according to the detection result.
4. The method for detecting the content of aconitic acid in pinellia ternata as claimed in claim 3, wherein: in step a, the solvent for ultrasonic extraction is water or 80% methanol.
5. The method for detecting the content of aconitic acid in pinellia ternata as claimed in claim 4, wherein: the dosage of water is 20-50mL per 1g of pinellia ternata powder.
6. The method for detecting the content of aconitic acid in pinellia ternata as claimed in claim 5, wherein: 50mL of water was used per 1g of pinellia tuber powder.
7. The method for detecting the content of aconitic acid in pinellia ternata as claimed in claim 3, wherein: in the step a, 0.1ml of phosphoric acid is used for every 25ml of supernatant; and/or the number of extractions with ethyl acetate is 5.
8. The method for detecting the content of aconitic acid in pinellia ternata as claimed in claim 3, wherein: in the step a, the ultrasonic extraction time is 15-120 minutes.
9. The method for detecting the content of aconitic acid in pinellia ternata as claimed in claim 8, wherein: the time for the ultrasonic extraction was 60 minutes.
10. The method for detecting the content of aconitic acid in pinellia ternata as claimed in claim 3, wherein: in step c, the specification of the chromatographic column is as follows: the inner diameter is 4.6mm, the length is 250mm, and the grain diameter of the filler is 5 mu m.
11. The method for detecting the content of aconitic acid in pinellia ternata as claimed in claim 10, wherein: the model of the chromatographic column is an Inertsil ODS-3C18 chromatographic column.
12. The method for detecting the content of aconitic acid in pinellia ternata as claimed in claim 3, wherein: the column temperature of the chromatographic condition is 25-35 ℃; the flow rate is 0.5-0.8 mL/min.
13. The method for detecting the content of aconitic acid in pinellia ternata as claimed in claim 12, wherein: the column temperature of the chromatographic conditions was 35 ℃; the flow rate was 0.8 mL/min.
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