CN113759055B - Method for establishing characteristic spectrum of rhizoma dioscoreae septemlobae test sample - Google Patents
Method for establishing characteristic spectrum of rhizoma dioscoreae septemlobae test sample 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
- G01N30/8634—Peak quality criteria
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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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
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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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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
The invention provides a method for establishing a characteristic spectrum of a rhizoma dioscoreae hypoglaucae test sample, which comprises the steps of obtaining the characteristic spectrum of the rhizoma dioscoreae hypoglaucae test sample by adopting ultra-high performance liquid chromatography; the test sample comprises at least 1 of rhizoma Dioscoreae Septemlobae decoction pieces, standard decoction and granule; the characteristic map at least comprises 5 characteristic peaks, the peak corresponding to tryptophan is taken as an S peak, and the relative retention time of each characteristic peak and the S peak is within +/-10% of a specified value; the specified values of the 5 characteristic peaks are as follows in sequence: 0.35, 0.72, 0.90, 1.00, 2.12. The method establishes the characteristic spectrums simultaneously suitable for the rhizoma dioscoreae hypoglaucae decoction pieces, the standard decoction and the formula particles, and can effectively compare and analyze the difference and the change from the rhizoma dioscoreae hypoglaucae decoction pieces to the characteristic spectrums of the formula particles; can be beneficial to the overall evaluation of the scientificity and rationality of the related process from the decoction pieces to the formula granules of the dioscorea spongiosa, and can be more beneficial to the overall control of the internal quality of the decoction pieces, the standard decoction and the formula granules of the dioscorea spongiosa.
Description
Technical Field
The invention relates to the field of ultra-high performance liquid chromatography, in particular to a method for establishing a characteristic spectrum of a dioscorea spongiosa yam rhizome test sample.
Background
The rhizoma Dioscoreae Septemlobae is dried rhizome of Dioscorea spongiosa J.Q.xi, M.Mizuno et W.L.ZHao, dioscorea batatas of Dioscoreaceae or Dioscorea batatas Futschauensis μm.M. line ex R.Kunth. It is listed as the "Shen nong Ben Cao Jing" as the "Zhong Pin". It is bitter and neutral in taste, and enters kidney and stomach meridians. Has effects of promoting diuresis, removing turbid pathogen, dispelling pathogenic wind, and removing arthralgia. The traditional Chinese medicine composition is clinically used for treating chylous stranguria, whitish and turbid urine, excessive leucorrhea, rheumatic arthralgia, joint discomfort and pain in waist and knees. In 'Chinese pharmacopoeia' 2020 edition, the medicinal material only controls characters, identification (thin layer, microscopy), inspection (extract, water content, total ash content) and the like, and has not been controlled by a characteristic map.
Most of the prior art methods for characteristic spectrum are used for measuring the content of specific characteristic components in rhizoma Dioscoreae Septemlobae, and cannot perform the overall evaluation of various characteristic components in rhizoma Dioscoreae Septemlobae. In the fingerprint spectrum research of part of rhizoma dioscoreae septemlobae medicinal materials, although a plurality of characteristic peaks corresponding to index components are marked, the separation degree between the characteristic peaks is poor, and the subsequent evaluation cannot be well carried out. Moreover, most of the standard decoction and the formula particles of the dioscorea spongiosa are water-soluble substances, and when the characteristic spectrum of the existing dioscorea spongiosa is measured, part of water-soluble components cannot be well extracted and detected, so that the fingerprint spectrum research of the existing dioscorea spongiosa is not suitable for the standard decoction and the formula particles of the dioscorea spongiosa.
Therefore, the existing detection method is difficult to effectively compare and analyze the difference and the change of the characteristic spectrums of the yam rhizome decoction pieces, the standard decoction and the formula granules, the transmission condition of the yam rhizome pharmacodynamic substance basis in the technical process from the raw materials to the formula granule finished products is difficult to deeply know, and the technical process from the yam rhizome decoction pieces to the formula granule finished products is difficult to integrally evaluate and control.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the problem that the existing detection method is difficult to effectively compare and analyze the difference and change of the characteristic spectrums of the yam rhizome decoction pieces, the standard decoction and the formula granules; thereby providing a method for establishing a characteristic spectrum of the test sample of rhizoma Dioscoreae Septemlobae.
A method for establishing characteristic spectrum of rhizoma Dioscoreae Septemlobae test sample comprises obtaining characteristic spectrum of rhizoma Dioscoreae Septemlobae test sample by ultra high performance liquid chromatography;
the test sample comprises at least 1 of rhizoma Dioscoreae Septemlobae decoction pieces, standard decoction and granule; the characteristic map at least comprises 5 characteristic peaks, the peak corresponding to tryptophan is taken as an S peak, and the relative retention time of each characteristic peak and the S peak is within +/-10% of a specified value; the specified values of the 5 characteristic peaks are as follows in sequence: 0.35, 0.72, 0.90, 1.00, 2.12.
The chromatographic conditions of the high performance liquid chromatography are as follows:
octadecylsilane chemically bonded silica is used as a filling agent; taking acetonitrile as a mobile phase A, taking a phosphoric acid solution with the volume concentration of 0.08-0.12% as a mobile phase B, and eluting according to the following gradient elution program, wherein the number of theoretical plates is not less than 10000 calculated according to a tryptophan peak;
the gradient elution procedure was:
in the chromatographic condition, the column temperature is 28-32 ℃ and the flow rate is 0.25ml/min.
The chromatographic column adopts Waters CORRTEC T3; the size of the chromatographic column is 2.1X 150mm,1.6um.
The standard decoction is extractive solution, concentrated solution or lyophilized powder.
When the test sample of the yam rhizome is yam rhizome decoction pieces, freeze-dried powder or formula particles, the process of preparing the yam rhizome test sample into the test sample solution comprises the following steps:
grinding rhizoma Dioscoreae Septemlobae sample, precisely weighing, precisely adding organic solvent at an amount of 50ml/g, weighing, ultrasonically treating, cooling, weighing, adding organic solvent to the reduced weight, shaking, filtering, and collecting the filtrate to obtain sample solution.
The power during ultrasonic treatment is 250W, and the frequency is 40kHz.
The organic solvent is a methanol solution with the volume concentration of 50%.
The technical scheme of the invention has the following advantages:
1. the invention provides a method for establishing a characteristic spectrum of a dioscorea spongiosa test sample, which establishes a characteristic spectrum simultaneously suitable for dioscorea spongiosa decoction pieces, standard decoction and formula granules, wherein the characteristic spectrum has 5 characteristic peaks including tryptophan, and the characteristic spectrum is ensured to simultaneously comprise organic phenolic acid components, amino acid components, steroid saponin components and other two components by limiting the relative retention time of the 5 characteristic peaks, thereby enhancing the specificity identification of the dioscorea spongiosa decoction pieces, the standard decoction and the formula granules, and realizing the control of the whole quality by limiting multiple components; therefore, the method can effectively compare and analyze the difference and the change of the characteristic spectrums of the yam rhizome decoction pieces, the standard decoction and the formula granules; can be beneficial to the overall evaluation of the scientificity and rationality of the related process from the decoction pieces to the formula granules of the dioscorea spongiosa, can be more beneficial to the overall control of the internal quality of the decoction pieces, the standard decoction and the formula granules of the dioscorea spongiosa, and ensures the clinical curative effect of the dioscorea spongiosa.
2. The establishment method provided by the invention further optimizes chromatographic conditions, not only optimizes a gradient elution program, but also adopts a wavelength switching mode to be matched with the gradient elution program, thereby effectively meeting the separation effect of each characteristic peak and ensuring that the separation degree of the obtained characteristic spectrum is good.
3. The characteristic spectrum established by the method of the invention fully reflects the characteristic peak information of the sample, and the method is stable, high in precision and good in reproducibility.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a characteristic diagram of solutions of standard decoction and reference substance in example 1 of the present invention;
FIG. 2 is a characteristic spectrum of rhizoma Dioscoreae Septemlobae decoction pieces, standard decoction, and formula granule in example 1 of the present invention;
FIG. 3 is a reference spectrum established by using the characteristic spectrum of the rhizoma Dioscoreae Septemlobae standard decoction in example 2 of the present invention;
FIG. 4 is a characteristic spectrum of rhizoma Dioscoreae Septemlobae decoction pieces, standard decoction, and formula granule in comparative example 1 of the present invention;
Detailed Description
The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.
The instrument comprises the following steps: waters ACQUITY
H-Class ultra-high performance liquid chromatograph; a PDA Detector; a TUV Detector Detector; empower 3 chromatography workstation; XP26 (mettler-toledo), BSA124S electronic balance (sydows scientific instrument (beijing) ltd), KQ-500DB ultrasonic cleaner (kunshan ultrasonic instrument ltd);
and (3) chromatographic column: waters CORTECS UPLC T3 (2.1X 150mm,1.6 um);
rhizoma Dioscoreae Septemlobae decoction pieces (batch number: 200520-322300-01, 200520-437300-02, 200525-438700-03, 200525-331100-04, 200525-331200-05, 200525-332700-06, 200525-332300-07, 200525-343100-08, 200525-343700-09, 200525-341100-10, 200525-342800-11, 200525-432100-12, 200525-432800-13, 200525-438600-15, 200525-437400-16, 200525-437600-17, 200525-432900-18);
rhizoma Dioscoreae Septemlobae standard decoction: placing the rhizoma Dioscoreae Septemlobae decoction pieces of the above batches into a casserole, soaking for 30 minutes, adding water 15 times of the decoction pieces in the first decoction, boiling with strong fire, decocting with slow fire for 30 minutes, filtering while hot, and rapidly cooling for use; adding water with the amount being 12 times of that of the decoction pieces into the second decoction, boiling the second decoction with strong fire, decocting the second decoction with slow fire for 20 minutes, filtering the second decoction while the second decoction is hot, and quickly cooling the second decoction for later use; the filtrates were combined and concentrated (65 ℃ C.) to a liquor to solids ratio of about 1:1 (relative density is 1.05-1.10 (50 ℃)), and freeze-drying to obtain the freeze-dried powder.
Rhizoma Dioscoreae Septemlobae formula granule: adding adjuvants into dry powder of rhizoma Dioscoreae Septemlobae to obtain granule (with batch number of KL200520-322300-01, KL200520-437300-02, KL 200525-438700-03);
tryptophan reference substances (batch No. 140686-201903), purity 99.9%, china institute for food and drug assay;
protodioscin reference substance (batch number: 55056-80-9), purity > 98%, chengdui Fengsi Biotech limited;
rhizoma Dioscoreae Septemlobae reference medicinal materials: batch number: 121545-201603, national institute for food and drug assay;
reagent: acetonitrile (Merck Liangyi, JB 094230), phosphoric acid (Fisher Scientific, 172387) as chromatographically pure; the water is distilled water; other reagents were analytically pure.
Example 1
A method for identifying characteristic spectrum of rhizoma Dioscoreae Septemlobae sample comprises the following steps:
1. preparation of a test solution:
respectively taking rhizoma Dioscoreae Septemlobae decoction pieces (lot number: 200520-322300-01), standard decoction (lot number: 200520-322300-01), and appropriate amount of formula granule (KL 200520-322300-01), grinding to about 0.5g, precisely weighing, placing in a conical flask with a plug, precisely adding 50% methanol 25ml, weighing, ultrasonic treating (power 250W, frequency 40 kHz) for 30 min, cooling, weighing again, supplementing lost weight with 50% methanol, shaking, filtering, and collecting filtrate to obtain sample solution.
Preparation of reference drug solution: collecting rhizoma Dioscoreae Septemlobae reference medicinal material, and preparing the subsequent filtrate by the same method as the above test solution to obtain reference medicinal material solution.
Preparation of control solutions: adding methanol into a proper amount of tryptophan reference substance to prepare a solution containing 20 μ g of tryptophan per 1ml as reference substance solution 1; taking appropriate amount of protodioscin as reference substance, adding methanol to obtain solution containing 0.2mg per lml as reference substance solution 2.
2. The detection process of the ultra-high performance liquid chromatography comprises the following steps:
precisely sucking 1 μ l of reference solution and sample solution respectively, injecting into ultra high performance liquid chromatograph, measuring by ultra high performance liquid chromatography, and recording chromatogram to obtain characteristic spectra of rhizoma Dioscoreae Septemlobae decoction pieces, standard decoction, and formula granule, as shown in fig. 1 and fig. 2.
The chromatographic conditions are as follows: octadecylsilane chemically bonded silica is used as a filler (Waters chromatographic column CORTECS UPLC T3,2.1 × 150mm, particle size 1.6 um); acetonitrile is taken as a mobile phase A, a phosphoric acid solution with the volume percentage of 0.1 percent is taken as a mobile phase B, gradient elution is carried out according to the specification of the following table 1, and the flow rate is 0.25ml per minute; the detection wavelengths are switched according to the time program in table 1; the column temperature is 30 ℃; the number of theoretical plates should not be less than 10000 calculated from tryptophan peaks.
TABLE 1 gradient elution
The characteristic spectrum of the rhizoma Dioscoreae Septemlobae sample detected by the detection method has 5 characteristic peaks corresponding to the retention time of 5 characteristic peaks in reference chromatogram peaks of reference medicinal material, the peak corresponding to the tryptophan reference chromatogram peak is the S peak, the relative retention time of each characteristic peak and the S peak is calculated, the relative retention time is within + -10% of the specified value, and the specified value is: 0.35 (peak 1), 0.72 (peak 2), 0.90 (peak 3), 2.12 (peak 5).
Example 2
The difference between this example and example 1 is that 18 batches of the yam rhizome standard decoction were tested, and the test results are shown in table 2.
TABLE 2
According to the detection results, the relative retention time of 18 batches of the rhizoma dioscoreae septemlobae standard decoction is within +/-10% of the specified value. A traditional Chinese medicine chromatogram fingerprint similarity evaluation system (2012 edition) is adopted to synthesize 18 batches of rhizoma Dioscoreae Septemlobae standard decoction samples, and a control spectrum of the characteristic spectrum of rhizoma Dioscoreae Septemlobae is established, as shown in figure 3.
Example 3
In this example, the precision verification of the chromatographic method in example 1 specifically includes:
1. repeatability verification
Taking 6 parts of a test solution of rhizoma Dioscoreae Septemlobae standard decoction (batch No. 200520-322300-01), obtaining its characteristic map according to the determination method in example 1, and calculating relative peak area and relative retention time by using peak No. 4 as reference peak. And calculates the RSD. The results are shown in tables 3 and 4.
TABLE 3
TABLE 4
From the above results, it can be seen that: the relative retention time of each characteristic peak and the RSD of the relative peak area are both less than 2.0 percent, which indicates that the method has good repeatability.
2. Intermediate precision experiment
A Waters UPLC H-Class TUV detector is adopted to take 6 parts of a test solution of a rhizoma Dioscoreae Septemlobae standard decoction (batch number: 200520-322300-01), a characteristic spectrum is obtained by measuring according to the method of the embodiment 1, the No. 4 peak is taken as a reference peak, the relative peak area and the relative retention time are calculated, and RSD is calculated. The results are shown in tables 5 and 6.
TABLE 5
TABLE 6
From the above results, it can be seen that: the relative retention time of each characteristic peak and the RSD of the relative peak area are both less than 5.0 percent, which indicates that the method has high intermediate precision.
3. Investigation of solution stability
The same standard decoction of rhizoma Dioscoreae Septemlobae (lot number: 200520-322300-01) was used as the test solution, and the test results are shown in Table 7 and Table 8, respectively, for 0,2,4,6,8, 10, 12, and 24 h.
TABLE 7
TABLE 8
The characteristic peaks in the sample are analyzed through the results, the relative retention time and the RSD of the relative peak area are both less than 2.0%, and the results show that the sample solution is stable within 24 h.
Example 4
The difference between this example and example 1 is that the chromatographic conditions are different, and specifically include:
1. difference in column temperature
The sample solution of the standard decoction of rhizoma Dioscoreae Septemlobae was subjected to characteristic spectrum detection according to the method in example 1 at column temperatures of 28 deg.C, 30 deg.C and 32 deg.C, respectively, and the detection results are shown in Table 9.
TABLE 9
The results show that: the method is suitable for column temperatures of 28-32 ℃.
2. Difference in concentration of the flowing amount B
The method of example 1 was used to perform characteristic spectrum detection on the test solution of the rhizoma Dioscoreae Septemlobae standard decoction using phosphoric acid solutions with concentrations of 0.08%, 0.10%, and 0.12%, respectively, and the detection results are shown in Table 10.
TABLE 10
The results show that: the method is suitable for the mobile phase B with the concentration of 0.08-0.12%.
Comparative example 1
Chromatographic conditions are as follows: gradient elution with acetonitrile (A) -water (B) was carried out to detect a wavelength of 208nm under the same conditions as in example 1, and the gradient elution procedure was as follows:
0-5min，5％→25％(A)；
5-20min，25％→30％(A)；
20-35min，30％→50％(A)；
35-36min，50％→60％(A)；
36-50min，60％→65％(A)。
the chromatogram obtained by detection is shown in FIG. 4.
As can be seen from the comparison of the results obtained in FIGS. 1-3 with FIG. 4, the number of peaks, the shape of peaks, and the degree of separation of the spectra obtained in examples 1-4 of the present invention are superior to those of comparative example 1, and the present invention can achieve the purpose of enhancing specificity identification and multi-component and overall quality control, and can be applied to the control of the production process of the Dioscorea tokoro Makino formula particles.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (7)
1. A method for establishing a characteristic spectrum of a rhizoma Dioscoreae Septemlobae test sample is characterized by comprising obtaining the characteristic spectrum of the rhizoma Dioscoreae Septemlobae test sample by ultra-high performance liquid chromatography;
the rhizoma Dioscoreae Septemlobae test sample comprises at least 1 of rhizoma Dioscoreae Septemlobae decoction pieces, standard decoction and granule; the characteristic map at least comprises 5 characteristic peaks, the peak corresponding to tryptophan is taken as an S peak, and the relative retention time of each characteristic peak and the S peak is within +/-10% of a specified value; the specified values of the 5 characteristic peaks are as follows in sequence: 0.35, 0.72, 0.90, 1.00, 2.12;
the chromatographic conditions of the ultra-high performance liquid chromatography are as follows:
octadecylsilane chemically bonded silica is used as a filler, the specification of a chromatographic column is 2.1 multiplied by 150mm, and the thickness is 1.6um; taking acetonitrile as a mobile phase A, taking a phosphoric acid solution with the volume concentration of 0.08-0.12% as a mobile phase B, and eluting according to the following gradient elution program, wherein the number of theoretical plates is not less than 10000 calculated according to a tryptophan peak;
The sample is extracted by adopting a methanol solution with the volume concentration of 50% as an organic solvent.
2. The method for establishing the characteristic spectrum of the rhizoma dioscoreae septemlobae test sample according to claim 1, wherein the gradient elution procedure can be replaced by:
。
3. The method for establishing the characteristic map of the rhizoma Dioscoreae Septemlobae test sample according to claim 1 or 2, wherein the chromatographic conditions comprise a column temperature of 28-32 deg.C and a flow rate of 0.24-0.26ml/min.
4. The method for establishing the characteristic spectrum of the rhizoma dioscoreae septemlobae test sample according to claim 1 or 2, wherein the chromatographic column adopts Waters CORRTEC T3; the size of the chromatographic column is 2.1X 150mm,1.6um.
5. The method for establishing the characteristic spectrum of the test sample of rhizoma Dioscoreae Septemlobae according to claim 1 or 2, wherein the standard decoction is an extract, a concentrate or a lyophilized powder.
6. The method for establishing the characteristic map of the dioscorea spongiosa thunb test sample according to claim 5, wherein when the dioscorea spongiosa thunb test sample is prepared from dioscorea spongiosa thunb decoction pieces, lyophilized powder or formula particles, the process for preparing the dioscorea spongiosa thunb test sample into the test sample solution comprises the following steps:
grinding rhizoma Dioscoreae Septemlobae sample, precisely weighing, precisely adding organic solvent at an amount of 25-125ml/g, weighing, ultrasonic treating, cooling, weighing again, adding the weight loss of organic solvent, shaking, filtering, and collecting the filtrate to obtain sample solution.
7. The method of claim 6, wherein the power of the sonication is 250W and the frequency is 40kHz.
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