CN109239251A - The measuring method of Lotrimin Sol Lotrimin HPLC-ELSD finger-print - Google Patents
The measuring method of Lotrimin Sol Lotrimin HPLC-ELSD finger-print Download PDFInfo
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- CN109239251A CN109239251A CN201811134324.9A CN201811134324A CN109239251A CN 109239251 A CN109239251 A CN 109239251A CN 201811134324 A CN201811134324 A CN 201811134324A CN 109239251 A CN109239251 A CN 109239251A
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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
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- 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
- 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
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Abstract
The present invention relates to the measuring methods of Lotrimin Sol Lotrimin HPLC-ELSD finger-print, the wherein measuring method, the following steps are included: the preparation of test solution, the preparation of reference substance solution, injection liquid chromatograph (evaporative light scattering detector) is measured, on the basis of standard finger-print, the Lotrimin Sol Lotrimin quality obtained with said determination method whether He Ge data, the method of the present invention is easy, fast, accurately, stablize, reliably, it can be used for the quality control of Lotrimin Sol Lotrimin sample, it can more comprehensively, it is objective, scientifically evaluate the quality of Lotrimin Sol Lotrimin, guarantee the validity of said preparation.
Description
Technical field
The present invention relates to traditional Chinese medicine fingerprint analysis methods, and in particular to Lotrimin Sol Lotrimin preparation finger measurement side
Method and its obtained Lotrimin Sol Lotrimin preparation finger.
Technical background
The composition of China's traditional Chinese medicine and compound preparation is sufficiently complex because its therapeutic effect be by whole coordination into
Capable.Therefore it should be carried out as an entirety when carrying out quality evaluation to it.However general quality standard is logical
The content height to some ingredient in Chinese medicine or compound is crossed to evaluate.It is difficult to control its inherent quality in this way.Therefore in order to mention
The Integral Characteristic of high and prominent Chinese medicine, establishes the quality control standard and evaluation model for meeting Chinese medicine feature.It could gradually accord with
" safely, effectively, stablize, is controllable " is really accomplished in the requirement for closing Chinese medicine and Chinese medicine development.
Lotrimin Sol Lotrimin be according to famous larynx section old docter of TCM Huang shen agriculture chief physician offer as a tribute the secret prescription handed down in the family from generation to generation development of nine generations and
At, be mainly used for acute and chronic laryngitis etc. card.Its quality standard is recorded in 2010 editions one page 1469 of " Chinese Pharmacopoeia ",
Middle discrimination test includes rheum officinale, Rhizoma Chuanxiong, Radix Glycyrrhizae, and assay detects the peimine and Peininine in fritillaria thunbergii.
Said preparation prescription includes peppermint, fritillaria thunbergii, Fructus Forsythiae, cicada slough, the sterculia seed, Rheum palmatum (processed with wine), Rhizoma Chuanxiong, catechu, campanulaceae, myrobalan
Effective component in 12 kinds of meat, Radix Glycyrrhizae and menthol raw material.
Existing detection method has: " measuring method and its standard finger-print of Lotrimin Sol Lotrimin preparation finger "
(patent), this method is that the fingerprint atlas detection method of gas-chromatography is established using gas chromatograph, in Lotrimin Sol Lotrimin
Volatile component is measured analysis.
It is newly-built in documents such as " 5 kinds of anthraquinone component contents in hplc simultaneous determination Lotrimin Sol Lotrimin "
Content method, using the means of high performance liquid chromatography-UV detector, main 7 kinds of ingredients for measuring source Rheum palmatum (processed with wine), including aloe
Rheum emodin, Rhein, rheum emodin, Chrysophanol, Physcion, Sennoside A and Sennoside B.But for Huang Shi sound in pharmacopeia
The detection method of ball quality evaluation is to utilize efficient liquid phase-ELSD detector, measurement peimine, the content of Peininine, and
Whole removing of having no way of evaluates said preparation, therefore establishes Lotrimin Sol Lotrimin HPLC-ELSD fingerprint spectrum method, on the whole
It goes to evaluate this medicine.
Summary of the invention
It is an object of the invention to: a kind of measuring method of Lotrimin Sol Lotrimin HPLC-ELSD finger-print is provided
The present invention provides a kind of Fast Evaluation said preparation by the research to Lotrimin Sol Lotrimin HPLC-ELSD fingerprint image
The method of middle composition quality compensates for the insufficient disadvantage of existing Quality Control Technology, controls the Lotrimin Sol Lotrimin quality of the pharmaceutical preparations
Technology is more perfect, also more scientific.
For this purpose, the present invention provides a kind of foundation of Lotrimin Sol Lotrimin gas chromatography standard finger-print and uses the fingerprint
The method that map is measured the Lotrimin Sol Lotrimin in production and selling.
Measuring method of the present invention, which is characterized in that steps are as follows:
(1) preparation of test solution: taking Lotrimin Sol Lotrimin, crushes, takes about 4g, accurately weighed, sets in conical flask, is added
85% methanol 50ml, ultrasound 1 hour, lets cool, and filters, is evaporated, and is dissolved, is transferred in separatory funnel, with acetic acid second with 25ml water
Ester extracts 3 times, each 25ml, and combined ethyl acetate extract liquor volatilizes, and residue is dissolved with methanol, is transferred to 5ml volumetric flask, adds
Methanol dilution shakes up to scale to obtain the final product.
(2) measuring method: accurate respectively to draw reference substance solution and each 20 μ l injection HPLC-ELSD color of test solution
Spectrometer, measurement, and record chromatic graph spectrum.
(3) gained chromatogram and standard finger-print are compareed, it is qualified product that similarity, which is greater than 0.75, and similarity evaluation is adopted
It is evaluated with " similarity evaluation 2004A editions ".
Wherein, the chromatographic condition is as follows:
Carbon octadecyl is fixed liquid-phase chromatographic column；
Mobile phase: -0.5% acetum (B) of methanol (A)
Flow velocity 0.8ml/min
30 DEG C of column temperature
Sample volume 20ul
ELSD condition:
Temperature: 80 DEG C；Gas flow rate: 1.2L/min
Preferably, the wherein preparation of test solution: taking Lotrimin Sol Lotrimin, crushes, takes about 4g, accurately weighed, sets taper
In bottle, 85% methanol 50ml is added, ultrasound 1 hour is let cool, and is filtered, is evaporated, and it is dissolved, is transferred in separatory funnel with 25ml water,
It is extracted with ethyl acetate 3 times, each 25ml, combined ethyl acetate extract liquor volatilizes, and residue is dissolved with methanol, is transferred to 5ml appearance
Measuring bottle adds methanol dilution to scale, shakes up to obtain the final product.
The present invention further provides the method for building up of standard finger-print, it is characterised in that: steps are as follows:
(1) preparation of test solution: taking multiple batches of Lotrimin Sol Lotrimin, crushes, takes about 4g, accurately weighed, sets conical flask
In, 85% methanol 50ml is added, ultrasound 1 hour is let cool, and is filtered, is evaporated, and is dissolved, is transferred in separatory funnel with 25ml water, is used
Ethyl acetate extracts 3 times, each 25ml, and combined ethyl acetate extract liquor volatilizes, and residue is dissolved with methanol, is transferred to 5ml capacity
Bottle, adds methanol dilution to scale, shakes up to obtain the final product.
(2) preparation of reference control solution: taking forsythin reference substance, Chrysophanol reference substance, Rhein reference substance appropriate,
Methanol is added, reference substance solution is made.
(3) measuring method: accurate respectively to draw reference substance solution and each 20 μ l injection HPLC-ELSD color of test solution
Spectrometer, measurement, and record chromatic graph spectrum.
(4) Lotrimin Sol Lotrimin HPLC-ELSD chromatogram of the multiple batches of qualification of gained is fitted to by a mark using computer
Quasi- finger-print；
Wherein, the chromatographic chromatographic condition of the HPLC-ELSD is as follows:
Carbon octadecyl is fixed liquid-phase chromatographic column；
Mobile phase: -0.5% acetum (B) of methanol (A)
Flow velocity 0.8ml/min
30 DEG C of column temperature
Sample volume 20ul
ELSD condition:
Temperature: 80 DEG C
Gas flow rate: 1.2L/min
The technical scheme is that obtained by screening, screening process is as follows:
1. instrument and reagent
1.1 instrument
Ten a ten thousandth electronic balances (METTLER TOLEDO), 1260 liquid chromatograph of Agilent, Alltech
3300ELSD, Agilent Eclipse SB-C18 4.6*250mm 5um chromatographic column.
1.2 reagent
Forsythin reference substance, Chrysophanol reference substance, Rhein reference substance, methanol, ethyl acetate
2. gas chromatography system condition:
Carbon octadecyl is fixed liquid-phase chromatographic column；
Mobile phase: -0.5% acetum (B) of methanol (A)
Flow velocity 0.8ml/min
30 DEG C of column temperature
Sample volume 20ul
ELSD condition:
Temperature: 80 DEG C
Gas flow rate: 1.2L/min
3. prepared by test solution
Lotrimin Sol Lotrimin is taken, crushes, takes about 4g, it is accurately weighed, it sets in conical flask, 85% methanol 50ml is added, ultrasound 1 is small
When, it lets cool, filters, be evaporated, dissolved with 25ml water, be transferred in separatory funnel, be extracted with ethyl acetate 3 times, each 25ml, close
And acetic acid ethyl acetate extract, it volatilizes, residue is dissolved with methanol, is transferred to 5ml volumetric flask, is added methanol dilution to scale, is shaken up i.e.
?.
4. prepared by reference substance solution
Forsythin reference substance, Chrysophanol reference substance, Rhein reference substance are appropriate, methanol are added, reference substance solution is made.Its
Middle forsythin reference substance concentration is 0.3125mg/ml, Chrysophanol reference substance concentration is 0.4981mg/ml, Rhein reference substance is dense
Degree is 0.5306mg/ml.
5. methodology validation
5.1 extraction times were investigated
3 parts of this product are weighed in parallel, each 4g is accurately weighed, sets in conical flask, 85% methanol 50ml is added, respectively ultrasound
10min, 20min, 30min, 1h, 2h are let cool, and filtering is evaporated, and are dissolved, are transferred in separatory funnel, with acetic acid second with 25ml water
Ester extracts 3 times, each 25ml, and combined ethyl acetate extract liquor volatilizes, and residue is dissolved with methanol, is transferred to 5ml volumetric flask, adds
Methanol dilution shakes up to scale to obtain the final product.
It is preferable by comparing experimental result discovery ultrasound 1h effect.Therefore, select ultrasound 1h as extraction time.
5.2 precision test
It takes with a test solution, continuously repeats 6 needle of sample introduction, investigate precision.Retain the result shows that shared peak is opposite
Time RSD is respectively less than 0.29%, and no more than 3.48%, the similarity repeated between 6 needle of sample introduction is relative peak area RSD
1.000 precision is good.Table 1, table 2 are that precision investigates result.
1 Precision test result of table (relative retention time)
2 Precision test result of table (relative peak area)
5.3 repeated
It weighs with a collection of 6 parts of test sample, according to sample solution preparation method, operation repetitive investigates repeatability.As a result table
Bright, shared peak relative retention time RSD is respectively less than 0.26%, and relative peak area RSD is no more than 3.38%, 6 part of sample room
Similarity is 0.999, and repeatability is good.Table 3, table 4 are that repeatability investigates result.
3 repetitive test result (relative retention time) of table
4 repetitive test result (relative peak area) of table
5.4 study on the stability
Same test solution is taken, respectively at 0h, 2h, 4h, 6h, 8h, 16h, injects liquid chromatograph for 24 hours.The result shows that
Shared peak relative retention time RSD is respectively less than 0.28%, and relative peak area RSD is respectively less than 3.38%, and similarity is 0.999 for examination
Product solution is stablized interior for 24 hours.Table 5, table 6 are that repeatability investigates result.
5 stability test result (relative retention time) of table
6 stability test result (relative peak area) of table
The measurement of 5.5 samples
10 batches of Lotrimin Sol Lotrimins are extracted by test sample extracting method, and are measured by the finger print measuring method,
Record each chromatogram.
6. data are analyzed
It is calculated, is obtained by the Chinese Pharmacopoeia committee " chromatographic fingerprints of Chinese materia medica similarity evaluation software " version in 2012
Every 10 batch similarity values.Sample similarity is 0.75~0.99.
Compared with prior art, improvement of the invention is:
1, fingerprint analysis method is directed to Lotrimin Sol Lotrimin multiple medicine material, multi-component feature, is analyzed on the whole,
Ensure that the medicine safely, effectively, controllably.
2, it is detected using efficient liquid phase-evaporative light scattering detector, is rung to " Chinese Pharmacopoeia " version Huang Shi in 2015
The supplement of sound ball mass analysis method, while being also the supplement for the existing analysis method of the kind.
Compared with prior art, the invention has the following advantages that
1, the present invention uses HPLC-ELSD method, shares peak in the Lotrimin Sol Lotrimin finger-print of foundation and summarizes 15, can have
The quality of characterization each ingredient of Lotrimin Sol Lotrimin of effect.
2, finger-print focuses on each correlation for constituting fingerprint characteristic peak, focuses on whole facial feature, both avoided
Total quality one-sidedness caused by due to measuring individual chemical ingredient, and reduce the possibility artificially handled for requisite quality
Property.The peak of Lotrimin Sol Lotrimin finger-print obtained by the method for the present invention is more, and peak shape is good, is easy to identify, and similitude is high, accurately and reliably.
3, this method have the advantages that precision, it is stability, reproducible and easy, quick, accurate, stablize, be reliable,
It can be used for the control of Lotrimin Sol Lotrimin quality.
4, this method can quickly and accurately identify the true and false superiority and inferiority of product.
Below with reference to embodiment and attached drawing, the present invention is described further.
Detailed description of the invention
Fig. 1 Lotrimin Sol Lotrimin standard finger-print
Fig. 2 Lotrimin Sol Lotrimin reference substance map
Fig. 3 Lotrimin Sol Lotrimin extraction comparison map
10 batches of finger-prints of Fig. 4 Lotrimin Sol Lotrimin
Specific embodiment
The present invention is further described with reference to embodiments, to make more detailed understanding to the present invention.
Embodiment 1
The preparation of step (1) test solution: taking Lotrimin Sol Lotrimin, crushes, takes about 4g, accurately weighed, sets in conical flask,
85% methanol 50ml is added, ultrasound 1 hour is let cool, and is filtered, is evaporated, and is dissolved with 25ml water, is transferred in separatory funnel, uses second
Acetoacetic ester extracts 3 times, each 25ml, and combined ethyl acetate extract liquor volatilizes, and residue is dissolved with methanol, is transferred to 5ml capacity
Bottle, adds methanol dilution to scale, shakes up to obtain the final product.
It is 0.3125mg/ml, greatly that step (2) reference substance solution preparation concentration, which is respectively as follows: wherein forsythin reference substance concentration,
Yellow phenol reference substance concentration is 0.4981mg/ml, Rhein reference substance concentration is 0.5306mg/ml.
Test solution, reference substance solution injecting chromatograph are obtained chromatogram by step (3).
The chromatographic condition of liquid chromatograph is as follows:
Carbon octadecyl is fixed liquid-phase chromatographic column；
Mobile phase: -0.5% acetum (B) of methanol (A)
Flow velocity 0.8ml/min, 30 DEG C of column temperature, sample volume 20ul
ELSD condition: temperature: 80 DEG C, gas flow rate: 1.2L/min
It is calculated, is compared by the Chinese Pharmacopoeia committee " chromatographic fingerprints of Chinese materia medica similarity evaluation software " version in 2012
The similarity of the finger-print of standard finger-print and said determination, similarity are qualification 0.75~0.99, are lower than 0.75
It is unqualified.
Embodiment 2
Determining fingerprint pattern is carried out to 170801 batch of Lotrimin Sol Lotrimin, the specific steps are as follows:
The preparation of step (1) test solution: taking Lotrimin Sol Lotrimin, crushes, takes about 4g, accurately weighed, sets in conical flask,
85% methanol 50ml is added, ultrasound 1 hour is let cool, and is filtered, is evaporated, and is dissolved with 25ml water, is transferred in separatory funnel, uses second
Acetoacetic ester extracts 3 times, each 25ml, and combined ethyl acetate extract liquor volatilizes, and residue is dissolved with methanol, is transferred to 5ml capacity
Bottle, adds methanol dilution to scale, shakes up to obtain the final product.
It is 0.3125mg/ml, greatly that step (2) reference substance solution preparation concentration, which is respectively as follows: wherein forsythin reference substance concentration,
Yellow phenol reference substance concentration is 0.4981mg/ml, Rhein reference substance concentration is 0.5306mg/ml.
Test solution, reference substance solution injecting chromatograph are obtained chromatogram by step (3).
The chromatographic condition of liquid chromatograph is as follows:
Carbon octadecyl is fixed liquid-phase chromatographic column；
Mobile phase: -0.5% acetum (B) of methanol (A)
Flow velocity 0.8ml/min, 30 DEG C of column temperature, sample volume 20ul
ELSD condition: temperature: 80 DEG C, gas flow rate: 1.2L/min
It is calculated, is compared by the Chinese Pharmacopoeia committee " chromatographic fingerprints of Chinese materia medica similarity evaluation software " version in 2012
The similarity of the finger-print of standard finger-print and said determination.
Test result: compared with standard diagram, similarity 0.86 meets and is not less than 170801 batch Lotrimin Sol Lotrimins
0.75 requirement.
Embodiment 3
Determining fingerprint pattern is carried out to 171003 batch of Lotrimin Sol Lotrimin, the specific steps are as follows:
The preparation of step (1) test solution: taking Lotrimin Sol Lotrimin, crushes, takes about 4g, accurately weighed, sets in conical flask,
85% methanol 50ml is added, ultrasound 1 hour is let cool, and is filtered, is evaporated, and is dissolved with 25ml water, is transferred in separatory funnel, uses second
Acetoacetic ester extracts 3 times, each 25ml, and combined ethyl acetate extract liquor volatilizes, and residue is dissolved with methanol, is transferred to 5ml capacity
Bottle, adds methanol dilution to scale, shakes up to obtain the final product.
It is 0.3125mg/ml, greatly that step (2) reference substance solution preparation concentration, which is respectively as follows: wherein forsythin reference substance concentration,
Yellow phenol reference substance concentration is 0.4981mg/ml, Rhein reference substance concentration is 0.5306mg/ml.
Test solution, reference substance solution injecting chromatograph are obtained chromatogram by step (3).
The chromatographic condition of liquid chromatograph is as follows:
Carbon octadecyl is fixed liquid-phase chromatographic column；
Mobile phase: -0.5% acetum (B) of methanol (A)
Flow velocity 0.8ml/min, 30 DEG C of column temperature, sample volume 20ul
ELSD condition: temperature: 80 DEG C, gas flow rate: 1.2L/min
It is calculated, is compared by the Chinese Pharmacopoeia committee " chromatographic fingerprints of Chinese materia medica similarity evaluation software " version in 2012
The similarity of the finger-print of standard finger-print and said determination.
Test result: compared with standard diagram, similarity 0.81 meets and is not less than 171003 batch Lotrimin Sol Lotrimins
0.75 requirement.
Embodiment 4
Determining fingerprint pattern is carried out to 171007 batch of Lotrimin Sol Lotrimin, the specific steps are as follows:
The preparation of step (1) test solution: taking Lotrimin Sol Lotrimin, crushes, takes about 4g, accurately weighed, sets in conical flask,
85% methanol 50ml is added, ultrasound 1 hour is let cool, and is filtered, is evaporated, and is dissolved with 25ml water, is transferred in separatory funnel, uses second
Acetoacetic ester extracts 3 times, each 25ml, and combined ethyl acetate extract liquor volatilizes, and residue is dissolved with methanol, is transferred to 5ml capacity
Bottle, adds methanol dilution to scale, shakes up to obtain the final product.
It is 0.3125mg/ml, greatly that step (2) reference substance solution preparation concentration, which is respectively as follows: wherein forsythin reference substance concentration,
Yellow phenol reference substance concentration is 0.4981mg/ml, Rhein reference substance concentration is 0.5306mg/ml.
Test solution, reference substance solution injecting chromatograph are obtained chromatogram by step (3).
The chromatographic condition of liquid chromatograph is as follows:
Carbon octadecyl is fixed liquid-phase chromatographic column；
Mobile phase: -0.5% acetum (B) of methanol (A)
Flow velocity 0.8ml/min, 30 DEG C of column temperature, sample volume 20ul
ELSD condition: temperature: 80 DEG C, gas flow rate: 1.2L/min
It is calculated, is compared by the Chinese Pharmacopoeia committee " chromatographic fingerprints of Chinese materia medica similarity evaluation software " version in 2012
The similarity of the finger-print of standard finger-print and said determination.
Test result: compared with standard diagram, similarity 0.88 meets and is not less than 171007 batch Lotrimin Sol Lotrimins
0.75 requirement.
The advantages of using HPLC-ELSD method:
(1) substance of not UV absorption is capable of detecting when using evaporative light scattering detector, it can be utmostly Huang
The substance of family name's sound ball separates well to be embodied.
(2) content assaying method of Lotrimin Sol Lotrimin is that peimine, peimisine are measured with HPLC-ELSD in pharmacopeia
Second.The finger-print also uses ELSD detector, the deficiency of detection method in the pharmacopeia supplemented to a certain extent.Simultaneously mostly at
The detection divided can preferably guarantee the quality of product.
Claims (3)
1. a kind of Lotrimin Sol Lotrimin HPLC-ELSD finger print measuring method, which is characterized in that steps are as follows:
(1) preparation of test solution: taking Lotrimin Sol Lotrimin, crushes, takes about 4g, accurately weighed, sets in conical flask, is added 85%
Methanol 50ml, ultrasound 1 hour, lets cool, and filters, is evaporated, and is dissolved with 25ml water, is transferred in separatory funnel, is extracted with ethyl acetate
It takes 3 times, each 25ml, combined ethyl acetate extract liquor volatilizes, and residue is dissolved with methanol, is transferred to 5ml volumetric flask, adds methanol
It is diluted to scale, shakes up to obtain the final product；
(2) measuring method: it is accurate respectively to draw reference substance solution and each 20 μ l injection HPLC-ELSD chromatograph of test solution,
Measurement, and record chromatic graph spectrum；
(3) gained chromatogram and standard finger-print are compareed, it is qualified product that similarity, which is greater than 0.75, and similarity evaluation uses
" similarity evaluation 2004A editions " is evaluated；
Wherein, the chromatographic condition is as follows:
Carbon octadecyl is fixed liquid-phase chromatographic column；
Mobile phase: -0.5% acetum (B) of methanol (A)
Flow velocity 0.8ml/min
30 DEG C of column temperature
Sample volume 20ul
ELSD condition:
Temperature: 80 DEG C；Gas flow rate: 1.2L/min.
2. finger print measuring method according to claim 1, which is characterized in that
The preparation of test solution: taking Lotrimin Sol Lotrimin, crushes, takes about 4g, accurately weighed, sets in conical flask, and 85% first is added
Alcohol 50ml, ultrasound 1 hour, lets cool, and filters, is evaporated, and is dissolved with 25ml water, is transferred in separatory funnel, is extracted with ethyl acetate 3
Secondary, each 25ml, combined ethyl acetate extract liquor volatilizes, and residue is dissolved with methanol, is transferred to 5ml volumetric flask, adds methanol dilution
To scale, shake up to obtain the final product.
3. the method for building up of standard finger-print described in claim 1, it is characterised in that: steps are as follows:
(1) preparation of test solution: taking multiple batches of Lotrimin Sol Lotrimin, crushes, takes about 4g, accurately weighed, sets in conical flask, adds
Enter 85% methanol 50ml, ultrasound 1 hour is let cool, and is filtered, is evaporated, and is dissolved with 25ml water, is transferred in separatory funnel, uses acetic acid
Ethyl ester extracts 3 times, each 25ml, and combined ethyl acetate extract liquor volatilizes, and residue is dissolved with methanol, is transferred to 5ml volumetric flask,
Add methanol dilution to scale, shake up to obtain the final product；
(2) preparation of reference control solution: taking forsythin reference substance, Chrysophanol reference substance, Rhein reference substance appropriate, is added
Reference substance solution is made in methanol；
(3) measuring method: it is accurate respectively to draw reference substance solution and each 20 μ l injection HPLC-ELSD chromatograph of test solution,
Measurement, and record chromatic graph spectrum；
(4) Lotrimin Sol Lotrimin HPLC-ELSD chromatogram of the multiple batches of qualification of gained a standard is fitted to using computer to refer to
Line map；
Wherein, the chromatographic chromatographic condition of the HPLC-ELSD is as follows:
Carbon octadecyl is fixed liquid-phase chromatographic column；
Mobile phase: -0.5% acetum (B) of methanol (A)
Flow velocity 0.8ml/min
30 DEG C of column temperature
Sample volume 20ul
ELSD condition:
Temperature: 80 DEG C
Gas flow rate: 1.2L/min.
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| CN113433235A (en) * | 2021-06-24 | 2021-09-24 | 无锡济煜山禾药业股份有限公司 | Method for determining content of platycodin D in Huangshi rattle tea |
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