CN110412197B - Method for constructing HPLC fingerprint spectrum of rhizoma polygonati medicinal material - Google Patents
Method for constructing HPLC fingerprint spectrum of rhizoma polygonati medicinal material Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8624—Detection of slopes or peaks; baseline correction
- G01N30/8631—Peaks
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8686—Fingerprinting, e.g. without prior knowledge of the sample components
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
Abstract
The invention relates to a method for constructing HPLC fingerprint of rhizoma polygonati medicinal material, which comprises the steps of preparing a test solution and selecting liquid phase conditions, and comprises the steps of taking rhizoma polygonati fine powder dried to constant weight, adding water and carrying out ultrasonic extraction; centrifuging the extractive solution at high speed, collecting supernatant, evaporating to dryness in evaporating dish in water bath, dissolving with 2-3mol/l hydrochloric acid, and evaporating to dryness in water bath at 90-95 deg.C while hydrolyzing and caramelizing; dripping methanol into the evaporating dish when the hydrochloric acid solution is completely evaporated to dryness to take away residual hydrochloric acid, and repeating for at least 2 times; dissolving the residue after evaporation with methanol, centrifuging, and filtering with microporous membrane; the invention has common peak value for different rhizoma polygonati medicinal materials, good precision, repeatability and stability, similarity between the rhizoma polygonati medicinal materials and a reference spectrum is more than 0.99, and the separation degree and the peak shape of an HPLC fingerprint spectrum are good.
Description
Technical Field
The invention belongs to a quality control method of a traditional Chinese medicine product, and particularly relates to a method for constructing an HPLC fingerprint of a rhizoma polygonati medicinal material.
Background
Rhizoma Polygonati is dried rhizome of Polygonatum sibiricum Red, Polygonatum kingianum Coll et al, Polygonatum cyrtonema Hua, Polygonatum cyrtonema, Liliaceae, Polygonatum sibiricum Red, Polygonatum cyrtonema Hua, and Polygonatum cyrtonema Red. The fingerprint spectrum of the traditional Chinese medicine can accurately reflect the real quality conditions of the traditional Chinese medicine and the preparation thereof by the characteristics of integrity, fuzziness, macroscopicity and the like.
When specific HPLC fingerprint chromatogram conditions are selected, the general principle means that the selected chromatogram conditions can enable various active ingredients contained in the traditional Chinese medicine to appear in the chromatogram to the maximum extent, the separation degree reaches the standard, and the peak shape is good.
In selecting the mobile phase, at least three different mobile phases are compared, and the mobile phase is selected to allow as many fingerprint peaks as possible and to achieve good separation, such as methanol-water, acetonitrile-0.5% acetic acid solution, etc. When selecting the elution mode, firstly referring to a possible isocratic elution mode of a related document, if isocratic elution is not feasible, then using gradient elution, considering the set gradient elution condition to come out at the fingerprint peak energy when performing gradient elution, and considering the drift of the baseline as little as possible on the basis of the separation degree meeting the requirement.
Rhizoma Polygonati contains saccharide, saponin, anthraquinone, alkaloid, cardiac glycoside, flavone, and amino acids. At present, the research on polygonatum polysaccharide and polygonatum saponin is relatively more. The saccharides contained in rhizoma Polygonati include mucilage, starch and sugar, wherein rhizoma Polygonati polysaccharides A, B and C have different molecular weights (more than 20 ten thousand). However, the polygonatum sibiricum produced in different producing areas has relatively different contents of different components, which shows that the quality of the polygonatum sibiricum produced in each producing area is different, and in order to accurately evaluate the quality of the polygonatum sibiricum, the HPLC fingerprint spectrum of the polygonatum sibiricum needs to be improved so as to achieve the best effect.
At present, no fingerprint spectrum or characteristic spectrum detection method exists in national standards (Chinese pharmacopoeia) of polygonatum, only extract and polysaccharide indexes are detected, the quality of polygonatum is difficult to be comprehensively reflected, the quality of products is not easy to control, and counterfeit products cannot be prevented. The construction method for researching the fingerprint of the polygonatum sibiricum is recorded in literature and comprises the steps of preparing a sample, wherein the method comprises the following steps: putting the rhizoma polygonati medicinal material into an oven for drying at 50 ℃ until the weight is constant, crushing, sieving by a 40-mesh sieve, precisely weighing 2g of the sample, adding 40ml of 70% ethanol, carrying out ultrasonic extraction for 30min, cooling, carrying out suction filtration, taking filtrate, adding 40ml of 70% ethanol into filter residue, carrying out ultrasonic extraction for 30min for the second time, cooling, carrying out suction filtration, combining the two extracting solutions, carrying out rotary drying, adding 10ml methanol into extract for constant volume, adding 100uL of 10g/L chitosan glacial acetic acid solution for overnight, filtering by a 0.22 mu m filter membrane, and taking the filtrate as a sample solution. The preparation method of the standard solution comprises accurately weighing appropriate amount of diosgenin, dissolving in methanol to obtain 113.9ug/ml reference solution, and filtering with 0.22 μm filter membrane. Chromatographic conditions for texture mapping, Waters 1525 binary high performance liquid chromatograph, Waters XB-C18 column (250mm × 4.6mm, 5 μm), Waters UV-2487 detector, in A: acetonitrile and B: water is used as a mobile phase, binary gradient elution is adopted, and the gradient program is as follows: 0-10min, 5% -10% A (v/v); 10-30min, 10% -35% A (v/v); 30-40min, 35% -60% A (v/v); 40-60min, 60% -100% A (v/v). The flow rate is 1mL/min, the column temperature is 30 ℃, the detection wavelength is 200nm, and the sample injection amount is 20 mu L. The above method is not sufficiently reproducible in stability.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for constructing an HPLC fingerprint of a polygonatum sibiricum medicinal material, which has better separation degree and peak shape.
The present invention comprises a method of,
1. preparing a test solution, namely taking 1g of fine powder dried to constant weight at 60 ℃ into a 50ml conical flask, and adding 20ml of water for ultrasonic extraction for 1 h; centrifuging the extractive solution at high speed, collecting supernatant 10ml, evaporating to dryness in evaporating dish with water bath, dissolving with 10ml 3mol/l hydrochloric acid, and evaporating to dryness in 95 deg.C water bath to hydrolyze and caramelize; when the hydrochloric acid solution is completely evaporated to dryness, dripping 2ml of methanol into the evaporating dish to take away residual hydrochloric acid, and repeating for 2 times; dissolving the residue after evaporation by using 10ml of methanol, centrifuging and filtering by using a microporous filter membrane to obtain the product;
2. liquid phase conditions of Agilent 1200LC HPLC (four-element pump G1311, autosampler G1329, temperature control box G1316A and DAD detector G4214); a chromatographic column: agilent Eclipse XDB-C18; detection wavelength: 290 nm; column temperature: 30 ℃; mobile phase: methanol/H2O; elution conditions: 0-15 min: 5-20% methanol, 15-20 min: 20-20% methanol, 20-25 min: 20-28% methanol, 25-32 min: 28-28% methanol, 32-60 min: 28-50% methanol, 60-70 min: 50-95% methanol.
The HPLC fingerprint construction method has the beneficial effects that the HPLC fingerprint construction method has common peak values for different rhizoma polygonati medicinal materials, the precision, the repeatability and the stability are good, the similarity between the HPLC fingerprint construction method and a reference map is more than 0.99, and the separation degree and the peak shape of the HPLC fingerprint are good.
Drawings
FIG. 1 is an HPLC chromatogram of Polygonatum sibiricum Red of example 1 (A-B: rhizoma Polygonati of different batches, C-D: Polygonatum sibiricum Red of different batches, E-F: Rheum emodin of different batches).
FIG. 2 is a comparison feature map of rhizoma Polygonati.
FIG. 3 is an HPLC chromatogram of rhizoma Polygonati extracted with methanol.
FIG. 4 is an HPLC chromatogram of rhizoma Polygonati extracted with mesityl oxide.
FIG. 5 is an HPLC chromatogram of the extraction of Polygonati officinalis rhizoma with diethyl ether.
FIG. 6 is an HPLC chromatogram of Experimental example 2.
FIG. 7 is an HPLC chromatogram of polygonatum polysaccharides after caramelization under water bath conditions.
FIG. 8 is an HPLC chromatogram of pyroglycation of polygonatum sibiricum polysaccharide in a state of being evaporated to dryness. (A: 3mol/L +75 ℃ C.; B: 3mol/L +85 ℃ C.; C: 3mol/L +95 ℃ C.; D: 4mol/L +95 ℃ C.; E: 5mol/L +95 ℃ C.; F: 6mol/L +95 ℃ C.).
FIG. 9 is a HPLC characteristic spectrum of 31 batches of rhizoma Polygonati medicinal materials.
Detailed Description
Example 1
The present invention comprises a method of,
1. preparing a test solution, namely taking 1g of fine powder dried to constant weight at 60 ℃ into a 50ml conical flask, and adding 20ml of water for ultrasonic extraction for 1 h; centrifuging the extractive solution at high speed, collecting supernatant 10ml, evaporating to dryness in evaporating dish with water bath, dissolving with 10ml 3mol/l hydrochloric acid, and evaporating to dryness in 95 deg.C water bath to hydrolyze and caramelize; when the hydrochloric acid solution is completely evaporated to dryness, dripping 2ml of methanol into the evaporating dish to take away residual hydrochloric acid, and repeating for 2 times; dissolving the residue after evaporation by using 10ml of methanol, centrifuging and filtering by using a microporous filter membrane to obtain the product;
2. liquid phase conditions of Agilent 1200LC HPLC (four-element pump G1311, autosampler G1329, temperature control box G1316A and DAD detector G4214); a chromatographic column: agilent Eclipse XDB-C18; detection wavelength: 290 nm; column temperature: 30 ℃; mobile phase: methanol/H2O; the flow rate was 1ml per minute; the amount of sample was 10. mu.L. The theoretical plate number is not less than 6000 calculated according to 5-hydroxymethylfurfural. Elution conditions: 0-15 min: 5-20% methanol, 15-20 min: 20-20% methanol, 20-25 min: 20-28% methanol, 25-32 min: 28-28% methanol, 32-60 min: 28-50% methanol, 60-70 min: 50-95% methanol.
And (4) measuring, namely injecting 10 mu l of each precision sample solution into a liquid chromatograph, and measuring to obtain the product. The test sample characteristic spectrum should present 9 characteristic peaks, and should correspond to 9 characteristic peaks in the reference substance chromatogram peak of the reference medicinal material, wherein peak 1 should be consistent with the retention time of the reference substance peak of the reference substance. The chromatograms of the samples from different batches are shown in figure 1. The reference characteristic spectrum of rhizoma Polygonati is shown in FIG. 2.
Experimental example 1
HPLC characteristic map
Extracting rhizoma Polygonati with solvent such as methanol, acetone, and diethyl ether, performing high performance liquid analysis, and preparing sample by collecting rhizoma Polygonati sample powder 2g dried at 60 deg.C to constant weight, adding extraction solvent 20ml (the extraction solvent is methanol, acetone and diethyl ether respectively), ultrasonic extracting for 30min, centrifuging methanol extraction supernatant at high speed, filtering with microporous membrane, introducing sample, analyzing, centrifuging acetone and diethyl ether extraction supernatant, collecting 12ml, spin-drying with rotary evaporator, dissolving with 1ml methanol, centrifuging at high speed, collecting supernatant, filtering with microporous membrane, and introducing sample for analysis. Detection wavelength: 210 nm; column temperature: 30 ℃; mobile phase: ACN/0.05% H3PO 4-H2O; elution conditions: 0-45 min: 20-90% ACN, 45-50 min: 90-95% ACN, 55-65 min: 95% ACN; sample introduction amount: 10 μ l, the HPLC chromatogram thereof is shown in FIGS. 3 to 5. As can be seen from FIGS. 3-5, the common peaks and the absorptions of rhizoma Polygonati samples in different batches and varieties are very small, and the extraction solution of rhizoma Polygonati is not suitable for HPLC fingerprint spectrum research.
Experimental example 2
Hydrolyzing rhizoma Polygonati polysaccharide, and performing liquid phase analysis on monosaccharide derivatization after hydrolysis, wherein the specific method is as follows.
Preparing polygonatum polysaccharide: putting 1g of rhizoma Polygonati sample in a 50ml conical flask, adding 20ml of water, performing ultrasonic extraction for 45min, centrifuging to obtain supernatant, adding 80ml of anhydrous ethanol, standing in a refrigerator at 4 ℃ for 12h, centrifuging, dissolving precipitate with 10ml of water, centrifuging to obtain supernatant, and spin-drying with a rotary evaporator to obtain rhizoma Polygonati polysaccharide.
Polysaccharide hydrolysis: the polysaccharide prepared above was taken, dissolved in 2ml water in a stoppered tube, added with 4ml of 2mol/L trifluoroacetic acid (TFA) solution, plugged, hydrolyzed in an oven at 105 ℃ for 6h, taken out and spun dry with a rotary evaporator, the precipitate was washed with MeOH (3ml) and spun dry, repeated 3 times, and excess TFA was taken away. Finally, dissolving the precipitate with 2ml of water, centrifuging, and taking the supernatant, namely the polysaccharide hydrolysate.
Derivatization: and (3) putting the hydrolysate into a 10ml test tube with a plug, adding 1ml of sodium hydroxide solution with the concentration of 0.3mol/L and 1.2ml of 1-phenyl-3-methyl-pyrazolone (PMP) solution with the concentration of 0.5mol/L, uniformly mixing and sealing the plug. The mixture is put into a water bath at 70 ℃ for reaction for 1h, taken out, cooled to room temperature, and added with 1ml of hydrochloric acid solution (0.3mol/L) to neutralize sodium hydroxide. Extracting with chloroform for three times (5ml × 3), collecting water layer, centrifuging, and collecting supernatant.
Liquid phase conditions: detection wavelength: 250 nm; column temperature: 30 ℃; mobile phase: in ACN/phosphate buffer (PH 6.8); elution conditions: 0-25 min: 15-30% ACN, 25-35 min: 30-90% ACN; sample introduction amount: 10 μ l.
After sample injection analysis (as shown in fig. 6), only 3 peaks after monosaccharide derivation are seen on the right side of the PMP peak except for the residual PMP peak, the method is complex to operate, and finally obtained chromatographic spectra are still few, so that the method is still difficult to be used as a fingerprint or characteristic spectrum of polygonatum sibiricum to control the quality of polygonatum sibiricum.
Experimental example 3
The method parameters are examined, and the key factor influencing hydrolysis and caramelization is found to be the process of adding hydrochloric acid for heating, so that the heating time, temperature and acid concentration can generate great influence on the experimental result, and the following methods are examined:
taking 1g of three parts of fine powder dried to constant weight at 60 ℃ into a 50ml conical flask, and adding 20ml of water respectively for ultrasonic extraction for 1 h. After the extracting solution is centrifuged at high speed, 5ml of supernatant is taken to be placed in a test tube with a plug, 5ml of hydrochloric acid with the concentration of 3mol/L is added to react in water bath with the temperature of 75 ℃, 85 ℃ and 95 ℃ for 30min, then the mixture is taken out, 5ml of NaOH with the concentration of 3mol/L is respectively dripped to neutralize the hydrochloric acid, and then the supernatant is taken to be centrifuged at high speed and filtered through a microporous filter membrane, and then the sample injection analysis is carried out. The result shows that the product is single under the reaction conditions of the three temperatures, and only 5-hydroxymethylfurfural is mainly generated. The results were not improved by changing the hydrochloric acid concentrations to 4, 5 and 6mol/L and shortening and lengthening the reaction time, and the chromatogram thereof is shown in FIG. 7.
Secondly, because the peak of the product generated by the caramelization reaction of the constant-temperature water bath is less, the caramelization is directly carried out in a method of reacting while evaporating in an evaporating dish by trying to control the temperature, and then the analysis is carried out. The specific operation method comprises the following steps: taking 1g of fine powder dried to constant weight at 60 ℃ into a 50ml conical flask, and adding 20ml of water for ultrasonic extraction for 1 h. Centrifuging the extractive solution at high speed, collecting supernatant 10ml, evaporating to dryness in evaporating dish with water bath, dissolving with 10ml hydrochloric acid, and placing the evaporating dish on water bath to allow hydrolysis and caramelization while evaporating to dryness. When the hydrochloric acid solution is completely evaporated to dryness, 2ml of methanol is dripped into the evaporating dish to take away residual hydrochloric acid, and the process is repeated for 2 times. The residue after evaporation to dryness was dissolved in 10ml of methanol, centrifuged, filtered through a microporous membrane and analyzed by sample injection. When the concentration of hydrochloric acid and the temperature of the water bath were examined, it was found from FIG. 8(A, B and C) that the number of liquid chromatography peaks was large when the temperature of the water bath was 95 ℃. As can be seen from FIG. 8(D, E and F), the chromatographic peak did not change much at a hydrochloric acid concentration of 4mol/L or 5mol/L, while the reaction was too vigorous, the caramelized product peak was too much and the absorption was weak when the concentration was increased to 6mol/L because the acid strength was too large. From this, it can be concluded that the HPLC chromatogram is optimal for a hydrochloric acid concentration of 3mol/L and a water bath temperature of 95 ℃, and is more suitable for quality control.
Experimental example 4
(3) Methodology investigation
And (3) precision test: an aliquot of a1 sample was prepared as in example 1 and analyzed six consecutive times under the chromatographic conditions described above, and the retention time and peak area were recorded. The retention time RSD of the 9 common peaks is measured to be 0.86%, 0.55%, 0.32%, 0.13%, 0.14%, 0.03%, 0.04%, 0.06% and 0.05% in sequence, the peak areas RSD are respectively 3.13%, 3.29%, 3.05%, 0.75%, 0.91%, 0.81%, 1.25%, 0.75% and 0.65%, and the precision is good.
And (3) repeatability test: 6 parts of A1 sample were prepared in parallel and assayed analytically under the liquid chromatographic conditions described above. The retention time RSD of the 9 common peaks is measured to be 0.33%, 0.23%, 0.26%, 0.21%, 0.24%, 0.14%, 0.15%, 0.14% in sequence, and the peak areas RSD are respectively 3.38%, 3.57%, 3.24%, 0.65%, 1.08%, 1.26%, 0.61%, 2.85%, and 2.31%, which indicates that the repeatability is good.
And (3) stability test: a1 sample solution is prepared, and the sample solution is injected and measured for 0h, 2h, 4h, 8h, 12h and 24h respectively, the retention time RSD of 9 common peaks is measured to be 0.20%, 0.14%, 0.12%, 0.08%, 0.10%, 0.04%, 0.06%, 0.29% and 0.08%, the peak area RSD is respectively 0.91%, 1.00%, 0.62%, 0.68%, 0.21%, 0.87%, 0.69%, 0.75% and 0.65%, and the stability is good.
Establishment of fingerprint
And (3) preparing 31 batches of collected rhizoma polygonati medicinal materials and 14 batches of rhizoma polygonati decoction pieces according to the methods under the sample preparation items, and then carrying out sample injection analysis according to the liquid phase conditions to obtain chromatograms of the rhizoma polygonati medicinal materials and the rhizoma polygonati decoction pieces. Introducing the chromatogram into traditional Chinese medicine chromatogram fingerprint similarity evaluation system software, respectively taking A1 and X1 as reference spectra and time window of 0.1, and respectively establishing characteristic spectra after automatically matching chromatogram peaks (figure 9). The similarity of the two maps is more than 0.99.
Claims (2)
1. A method for constructing an HPLC fingerprint of a rhizoma polygonati medicinal material is characterized by comprising the following steps:
(1) preparing a test solution, namely adding water into the fine powder of the rhizoma polygonati dried to constant weight for ultrasonic extraction; centrifuging the extractive solution at high speed, collecting supernatant, evaporating to dryness in evaporating dish in water bath, dissolving with 2-3mol/l hydrochloric acid, and placing the evaporating dish in 90-95 deg.C water bath to hydrolyze and caramelize; dripping methanol into the evaporating dish when the hydrochloric acid solution is completely evaporated to dryness to take away residual hydrochloric acid, and repeating for at least 2 times; dissolving the residue after evaporation with methanol, centrifuging, and filtering with microporous membrane;
(2) liquid phase conditions detection wavelength: 290nm, column temperature: 30 ℃, mobile phase: methanol/H2O; elution conditions, 0-15 min: 5-20% methanol, 15-20 min: 20-20% methanol, 20-25 min: 20-28% methanol, 25-32 min: 28-28% methanol, 32-60 min: 28-50% methanol, 60-70 min: 50-95% methanol;
the liquid phase conditions also include American Agilent 1200LC HPLC; a chromatographic column: agilent Eclipse XDB-C18.
2. The method for constructing HPLC fingerprint of rhizoma Polygonati as claimed in claim 1, wherein the sample solution is prepared by collecting 1g of fine powder dried at 60 deg.C to constant weight in a 50ml conical flask, adding 20ml of water, and performing ultrasonic extraction for 1 h; centrifuging the extractive solution at high speed, collecting supernatant 10ml, evaporating to dryness in evaporating dish with water bath, dissolving with 10ml 3mol/l hydrochloric acid, and placing the evaporating dish on 95 deg.C water bath to hydrolyze and caramelize; when the hydrochloric acid solution is completely evaporated to dryness, dripping 2ml of methanol into the evaporating dish to take away residual hydrochloric acid, and repeating for 2 times; dissolving the residue after evaporation with 10ml methanol, centrifuging, and filtering with microporous membrane.
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