CN111751465B - Rapid quantitative screening method and application of liquorice antioxidant active ingredients - Google Patents
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Abstract
The invention relates to a rapid quantitative screening method of liquorice antioxidant active ingredients and application thereof, belonging to the technical field of traditional Chinese medicine quality evaluation and control. Aiming at the problems of quality control of the drug effect of the liquorice at the present stage, a method for quickly screening active ingredients and quickly and quantitatively measuring the antioxidant activity of each ingredient is established by utilizing the antioxidant activity of the liquorice, the method can quickly screen the antioxidant active ingredients in the traditional Chinese medicine liquorice while analyzing chemical ingredients, quantitatively evaluate the antioxidant activity of each ingredient, research and optimize the quality evaluation method of the liquorice, realize the correlation between quality evaluation and drug effect, more truly reflect the quality of decoction pieces, and provide certain data support for the research of the base of the antioxidant substances of the liquorice.
Description
Technical Field
The invention relates to a rapid quantitative screening method of liquorice antioxidant active ingredients and application thereof, belonging to the technical field of traditional Chinese medicine quality evaluation and control.
Background
The Glycyrrhrizae radix is dried root and rhizome of Glycyrrhiza uralensis Fisch, Glycyrrhiza inflata Bat or Glycyrrhiza glabra L of Leguminosae, and is mainly distributed in northeast, North China, Gansu, Xinjiang, etc. The liquorice has the effects of tonifying spleen and qi, clearing heat and detoxicating, eliminating phlegm and stopping cough, relieving spasm and pain and harmonizing the drugs, is commonly used for treating symptoms such as weakness of spleen and stomach, lassitude and hypodynamia, palpitation and shortness of breath, cough and profuse sputum, spasm and pain of epigastrium and four limbs and the like in clinic, and can simultaneously relieve drug toxicity and intensity. Modern pharmacological studies show that liquorice has strong antioxidant activity and is widely applied to a plurality of fields as a natural antioxidant at present. And various pharmacological activities of anti-inflammation, sterilization, anti-aging and the like are closely related to the antioxidant activity of the compound. The antioxidant active ingredients in licorice, which have been reported, include many kinds of compounds such as flavone, polysaccharide and triterpene.
At present, increasingly rich component information can be obtained for liquorice chemical component analysis including GC-MS, HPLC content determination, HPLC fingerprint, HPLC-MS technology and the like, but because the pharmacodynamic substance basis of liquorice is not clear, the index components of quality control are not related to the efficacy, so that the content of the index components cannot really represent the quality of the liquorice.
Disclosure of Invention
The invention aims at the problem that the quality evaluation method of the liquorice at the present stage and the evaluation index are lack of correlation with the drug effect, and utilizes the antioxidant activity of the liquorice to establish a rapid screening method of active ingredients.
A rapid quantitative screening method of liquorice antioxidant active ingredients comprises the following steps:
(1) preparation of a test solution: crushing dried liquorice decoction pieces, sieving the crushed liquorice decoction pieces with a 60-mesh sieve, and adding methanol, wherein the ratio of the liquorice to the methanol is 1 g: 20mL, carrying out ultrasonic treatment, and filtering the filtrate through a 0.45 mu m microporous filter membrane;
(2) preparation of Vc control solution: preparing a stock solution from an L (+) -ascorbic acid standard substance, and storing the stock solution in a refrigerator at 4 ℃ for later use;
(3) HPLC-UV-DPPH on-line system:
chromatographic conditions of an HPLC system: 4.6X 250 mm, 5 μm XDB-C18A chromatographic column, the column temperature is 30 ℃; gradient elution is carried out on mobile phase acetonitrile (A) -0.2% formic acid water solution (B), and the wavelength of a detector is 254 nm;
chromatographic conditions of post-column free radical analysis system: the mobile phase is DPPH-methanol solution, the detection wavelength is 517 nm, and the post-column temperature is 30 ℃;
(4) mass spectrum conditions: the mobile phase adopts three-way flow division; electrospray positive ion mode; the full scanning range m/z is 100-1000; capillary voltage 4000V; introducing dry gas at the temperature of 350 ℃; the cracking voltage is 300V; the taper hole voltage is 65V, and the atomizing gas pressure is 30 psi;
(5) obtaining the characteristic map of the liquorice, and obtaining the antioxidant active ingredients of the liquorice and the antioxidant activity of each active ingredient.
The gradient elution condition in the step (4) is as follows: 0-10 min, 15% -25% A; 10-20.3 min, 25% -30% A; 20.3-70 min, 30-70% A; 70-75 min, 70% -15% A.
The concentration of the stock solution in the step (3) is 0.05 mg/mL-1。
The rapid quantitative screening method is used for controlling and evaluating the quality of the liquorice decoction pieces.
The licorice effect atlas obtained by the post-column analysis system can be used for screening to obtain licorice antioxidant active ingredients (the expression in the atlas is a peak inversion); according to the peak areas of the peaks of the adverse peaks of the effect maps, the difference of the antioxidant activity of the liquorice in different batches can be visually and objectively compared; identifying the antioxidant active ingredients according to mass spectrum information, so that the composition of the antioxidant active ingredients can be determined; the DPPH clearance rate of each antioxidant active component can be calculated simultaneously by combining the peak area of the reference Vc, the sample concentration and the DPPH clearance rate.
The invention has the advantages of
1. Rapidly detecting multiple antioxidant active ingredients of licorice
The method disclosed by the invention is adopted to realize rapid screening of the antioxidant active ingredients in the liquorice decoction pieces, and the screened antioxidant ingredients are identified by combining HPLC-TOF/MS, so that 7 antioxidant active compounds in the liquorice are determined, namely avermectin, 8-isopentenyl naringenin, yellow lupin ketoneferone, hemiglycyrrhiza isoflavone B, 3',4' -dimethyl-3-hydroxy-6-methylflavone, glycyronin E and glycyronin H.
2. A two-dimensional map related to chemical components and antioxidant activity of liquorice and processed liquorice decoction pieces thereof is established, on one hand, rich chemical component information (figure 2) can be obtained, and antioxidant active components (peak inversion in figure 3) in liquorice can be synchronously screened and determined, as can be seen from figure 3, 7 antioxidant active components in 8 batches of liquorice samples are shown as peak inversion at the corresponding time of appearance of the antioxidant active components, and the method is proved to be applicable to screening of the antioxidant active components of the liquorice. The correlation between the peak inversion area and the oxidation resistance of the detected sample is determined by the online effect spectrum peak inversion principle (the DPPH clearance of different batches of liquorice detected in the table 2 and the peak area of each batch of liquorice peak inversion detected in the figure 3 are in positive correlation, which can be proved), so that the method can simultaneously and intuitively evaluate the difference of the oxidation resistance of different batches of liquorice decoction pieces.
3. And (3) correlating the peak area of an online spectrum and the DPPH clearance of VC by taking Vc as a reference, calculating the concentration of Vc corresponding to each component in the measured licorice sample according to the peak area of each spectrum peak in the licorice sample, wherein CVc/AVc = C component to be measured/A component to be measured, and converting the DPPH clearance under the condition by combining the DPPH clearance of Vc under the concentration to obtain the DPPH clearance results of all active components detected under the condition.
4. The method is time-saving and labor-saving, and can complete the analysis of the composition of the liquorice decoction pieces, the screening of the antioxidant active ingredients, the evaluation of the whole antioxidant activity of the decoction pieces and the determination of the DPPH clearance rate of each active ingredient in the decoction pieces at the same time through one-time analysis. The problem that the existing quality evaluation method is irrelevant to the drug effect is solved to a certain extent. The detection results of a plurality of batches of decoction pieces show that the method has good stability and can be popularized and applied as a new quality evaluation method for liquorice.
Drawings
FIG. 1 is a graph of Vc antioxidant effect of example 1;
FIG. 2 is the fingerprint obtained in example 1;
FIG. 3 is the fingerprint of antioxidant effect of licorice obtained in example 1 (1-7 are avermectin, 8-isopentenylnaringenin, luteolin, hemiglycyrrhiza isoflavone B, 3',4' -dimethyl-3-hydroxy-6-methylflavone, glycyronin E and glycyronin H, respectively);
FIG. 4 is the total ion flow diagram of mass spectrum of Glycyrrhiza uralensis of example 1;
FIG. 5 is an HPLC chromatogram of Glycyrrhiza uralensis measured in comparative example 2.
Detailed Description
Example 1
Preparation of test solution Glycyrrhrizae radix sample powder of different production places 0.75 g each is weighed precisely, placed in a conical flask with a stopper, precisely added with methanol 15 mL, sealed, ultrasonically treated for 30 min, filtered, the filtrate is passed through 0.45 μm microporous membrane, and stored in a refrigerator at 4 deg.C for use.
Preparation of DPPH solution A DPPH standard is precisely weighed, methanol is added to the scale, and the solution is prepared to have the solubility of 80 mu mol.L-1The DPPH methanol solution is stored in a refrigerator at 4 ℃ for later use.
Preparation of Vc control solution: weighing appropriate amount of L (+) -ascorbic acid standard substance, weighing, adding distilled water to obtain a concentration of 0.05 mg/mL-1The stock solution is stored in a refrigerator at 4 ℃ for later use.
HPLC-UV-DPPH on-line system chromatographic condition HPLC system chromatographic condition: agilent Eclipse XDB-C18Chromatography column (4.6X 250 mm, 5 μm), column temperature 30 deg.C, flow rate 0.8 mL/min-1The amount of the sample was 10. mu.L. The mobile phase acetonitrile (A) -0.2 percent formic acid water solution (B) is eluted in a gradient way (0-10 min, 15-25 percent A, 10-20.3 min, 25-30 percent A, 20.3-70 min, 30-70 percent A, 70-75 min, 70-15 percent A), and the wavelength of a detector is 254 nm.
Chromatographic conditions of post-column free radical analysis system: the mobile phase is 80 mu mol.L-1DPPH-methanol solution, 0.8 mL. min-1The detection wavelength is 517 nm, and the post-column temperature is 30 ℃.
Mass spectrum conditions: the mobile phase is divided to 0.27 mL/min by a tee-1(ii) a Electrospray positive ion mode; the full scanning range m/z is 100-1000; capillary voltage 4000V; volume flow of drying gas 8L min-1At the temperature of 350 ℃; the cracking voltage is 300V; the cone voltage was 65V and the atomizing gas pressure was 30 psi.
The data obtained by HPLC-TOF/MS are analyzed by using the software Qualitive analysis B06.00 analysis software carried by an ESI-TOF/MS system. Through comparison and analysis of ultraviolet absorption spectrum, online spectrum and mass spectrum information of liquorice, retention time and accurate molecular weight of each compound, and reference to relevant documents, 7 active substances are identified in total. (in FIG. 3, Nos. 1-7 are Avalomogen, 8-isopentenyl naringenin, luteolin, hemiglycyrrhiza isoflavone B, 3',4' -dimethyl-3-hydroxy-6-methylflavone, glycyronin E and glycyronin H, respectively)
Taking licorice root 1 as an example, the DPPH clearance rate calculation results of the components are shown in Table 1:
TABLE 1 DPPH clearance determination results of 7 antioxidant active ingredients of raw licorice
Comparative example 1
DPPH clearance rate of liquorice decoction pieces
1 preparation of test solutions
Taking about 0.25 g of licorice powder (screened by a 60-mesh sieve), precisely weighing, placing in a conical flask with a plug, precisely adding 25 mL of methanol, sealing the plug, weighing, carrying out ultrasonic treatment (power 250W and frequency 40 kHz) for 30 min, cooling, weighing again, supplementing the weight loss by using methanol, shaking up, filtering, and taking a subsequent filtrate to obtain the liquorice powder.
Preparation of 2 DPPH solution
Taking a proper amount of DPPH standard substance, precisely weighing, adding methanol to prepare solution containing 0.2663 mu mol of DPPH per 1 mL, and storing in a refrigerator at 4 ℃ for later use.
3 determination of semi-inhibitory concentration of Glycyrrhiza solution
Taking sample solution, diluting to solubility of 10.00 mg/mL-1，2.00 mg·mL-1，1.00 mg·mL-1，0.80 mg·mL-1，0.40 mg·mL-1，0.20 mg·mL-1，0.10 mg·mL-1，0.04 mg·mL-1The sample solution of (4) for use. 2 mL of each dilution was placed in an EP tube, and 2 mL of 2.663X 10-1. mu. mol/mL was added-1Shaking the solution of DPPH in methanol, placing the solution in the dark for reaction for 30 min, and measuring the absorbance A at 517 nm by using a microplate readeri(ii) a Blank control group A was also set0(methanol solution instead of sample diluent) and sample background group Aj(methanol solution instead of DPPH. solution), aboveThe experiment was repeated three times, averaged and the DPPH-clearance and semi-inhibitory solubility (IC) calculated50). The concentration of the drug (mg. mL) was measured by this method-1) Dpph.clearance at 10.00, 2.00, 1.00, 0.80, 0.40, 0.20, 0.10, 0.04 was 98.38%, 74.36%, 62.55%, 51.71%, 50.95%, 45.07%, 44.88%, 44.74%, respectively; IC (integrated circuit)50=0.00024 g·mL-1。
4 Glycyrrhiza uralensis DPPH & clearance assay
Respectively weighing about 0.25 g of Glycyrrhrizae radix in different batches, precisely weighing, placing in a conical flask with a plug, precisely adding 25 mL of methanol solution, sealing the plug, ultrasonically treating for 30 min, cooling, filtering, and collecting the filtrate for use. Precisely measuring 0.6 mL of the licorice medicinal material extract in different producing areas, putting the extract in a 25 mL measuring flask, and adding methanol to a constant volume to reach scales. The absorbance at 517 nm was measured according to the "3" method, based on the IC obtained50As a result, the clearance to DPPH was calculated.
TABLE 2 DPPH clearance test results of raw and roasted liquorice
Comparative example 1 the antioxidant activity of the samples was evaluated by measuring the DPPH clearance of different batches of licorice samples by a microplate reader. On one hand, the method is complicated in operation process, and in addition, the method only obtains the evaluation result of the total antioxidant activity of the decoction pieces, and the composition of the liquorice, the information of the antioxidant active ingredients and the antioxidant activity of each active ingredient cannot be clarified.
Comparative example 2
Preparation of test solution dried Glycyrrhrizae radix decoction pieces are pulverized, sieved with 60 mesh sieve, and Glycyrrhrizae radix samples of different production places are taken 0.75 g each, weighed precisely, placed in a conical flask with a plug, added with 15 mL methanol precisely, sealed, treated with ultrasound for 30 min, filtered, and the filtrate is passed through 0.45 μm microporous membrane, and stored in a refrigerator at 4 deg.C for use.
Chromatographic conditions are as follows: agilent Eclipse XDB-C18Chromatography column (4.6X 250 mm, 5 μm), column temperature 30 deg.C, flow rate 0.8 mL/min-1The amount of the sample was 10. mu.L. The mobile phase acetonitrile (A) -0.2 percent formic acid water solution (B) is eluted in a gradient way (0-10 min, 15-25 percent A, 10-20.3 min, 25-30 percent A, 20.3-70 min, 30-70 percent A, 70-75 min, 70-15 percent A), and the wavelength of a detector is 254 nm. The results are shown in FIG. 5.
In comparative example 2, the quality of the liquorice decoction pieces is evaluated by an HPLC (high performance liquid chromatography) fingerprint spectrum method, and although the method has a plurality of detected components, whether the detected components are pharmacodynamic components and the activity of the components cannot be determined, so that the defect that the existing quality evaluation method is not strong in correlation with the pharmacodynamic effect cannot be overcome, and the quality of the decoction pieces cannot be really evaluated.
Claims (3)
1. A rapid quantitative screening method for liquorice antioxidant active ingredients is characterized by comprising the following steps:
(1) preparation of a test solution: crushing dried liquorice, sieving by a 60-mesh sieve, adding methanol, wherein the ratio of the liquorice to the methanol is 1 g: 20mL, carrying out ultrasonic treatment, and filtering the filtrate through a 0.45 mu m microporous filter membrane;
(2) preparation of Vc control solution: preparing a stock solution from an L (+) -ascorbic acid standard substance, and storing the stock solution in a refrigerator at 4 ℃ for later use;
(3) HPLC-UV-DPPH on-line system:
chromatographic conditions of an HPLC system: 4.6X 250 mm, 5 μm XDB-C18A chromatographic column, the column temperature is 30 ℃; the mobile phase A is acetonitrile, the mobile phase B is 0.2 percent formic acid water solution, gradient elution is carried out, and the wavelength of a detector is 254 nm;
chromatographic conditions of post-column free radical analysis system: the mobile phase is DPPH-methanol solution, the detection wavelength is 517 nm, and the post-column temperature is 30 ℃;
(4) mass spectrum conditions: the mobile phase adopts three-way flow division; electrospray positive ion mode; the full scanning range m/z is 100-1000; capillary voltage 4000V; introducing dry gas at the temperature of 350 ℃; the cracking voltage is 300V; the taper hole voltage is 65V, and the atomizing gas pressure is 30 psi;
(5) obtaining a liquorice characteristic map to obtain liquorice antioxidant active ingredients and antioxidant activity of each active ingredient;
the DPPH clearance rate of each antioxidant active component can be calculated simultaneously by combining the peak area, the sample concentration and the DPPH clearance rate of the Vc reference substance;
the antioxidant activity is Avalomoesin, 8-isopentenyl naringenin, WEITONE of yellow lupin, hemi-licoisoflavone B, 3',4' -dimethoxy-3-hydroxy-6-methylflavone, GANOSINE E and GANOSINE H;
the gradient elution condition in the step (3) is as follows: 0-10 min, the concentration of the mobile phase A is 15-25%; 10-20.3 min, the concentration of the mobile phase A is 25% -30%; 20.3-70 min, the concentration of the mobile phase A is 30-70%; 70-75 min, and the concentration of the mobile phase A is 70-15%.
2. The rapid quantitative screening method according to claim 1, wherein the stock solution in step (2) has a concentration of 0.05 mg-mL-1。
3. Use of the rapid quantitative screening method of claim 1 to evaluate the quality of licorice.
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