CN110231418A - A kind of method of Multiple components content in HPLC method separation determination ageratum oral liquid - Google Patents
A kind of method of Multiple components content in HPLC method separation determination ageratum oral liquid Download PDFInfo
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Abstract
The invention belongs to field of pharmaceutical preparations, are related to the method for quality control of ageratum oral liquid, and in particular to a kind of method of Multiple components content in HPLC method separation determination ageratum oral liquid.The present invention provides a kind of method of Multiple components content in HPLC method separation determination ageratum oral liquid, the chromatographic column that the HPLC method uses is mixed in a certain ratio with solution A and solution B and is eluted for mobile phase using silica matrix as filler；The solution A is acetonitrile, and the solution B is phosphoric acid water；The ingredient includes one of glycycoumarin, isoliquiritigenin, celery sugar liquiritin, narirutin, liquiritin, nobiletin or a variety of.Method of the invention is simple, sensitive, accuracy is high, can make up the defect that the prior art is not enough to illustrate component content in ageratum oral liquid, effectively ensure the quality of ageratum oral liquid.
Description
Technical field
The invention belongs to field of pharmaceutical preparations, are related to the method for quality control of ageratum oral liquid, and in particular to a kind of
The method of Multiple components content in HPLC method separation determination ageratum oral liquid.
Background technique
Ageratum oral liquid is a kind of Chinese patent drug, have inducing diaphoresis dampness elimination, qi-regulating and it is middle the effect of.Chinese Pharmacopoeia first
It records, prescription is by rhizoma atractylodis, Cortex Magnoliae Officinalis, Poria cocos, dried pinellia, patchouli oil, dried orange peel, the root of Dahurain angelica, the shell of areca nut, extract of licorice root and perilla leaf
Oil composition, pharmacopeia also describe the high-efficiency liquid chromatography method for detecting of Cortex Magnoliae Officinalis, dried orange peel and perilla leaf oil simultaneously.In addition, existing text
Offer in data, Yu Jiawen et al. establish while measuring aurantiamarin in ageratum oral liquid, narirutin, honokiol,
Magnolol, liquiritin, ammonium glycyrrhetate content UPLC analysis method, to control dried orange peel in preparation, Cortex Magnoliae Officinalis and extract of licorice root；Wang Jiao
Et al. establish while measuring aurantiamarin in ageratum oral liquid, Imperatorin, Isomperatorin, magnolol, honokiol,
The HPLC analysis method of rhizoma atractylodis cellulose content.The content that the above technical manual and disclosed documents and materials are recorded is not enough to illustrate the leaves of pulse plants
The content of ingredient in fragrant positive invigorating oral liquid.
Therefore, the present invention establishes a kind of HPLC analysis method to measure many indexes ingredient in ageratum oral liquid,
The present invention can provide scientific experiment foundation for the foundation of ageratum oral liquid global quality control appraisement system.
Summary of the invention
In consideration of it, one of the object of the invention, it is to provide a variety of in a kind of HPLC method separation determination ageratum oral liquid
Component content.
A kind of method of Multiple components content in HPLC method separation determination ageratum oral liquid, what the HPLC method used
Chromatographic column is mixed in a certain ratio with solution A and solution B and is eluted for mobile phase using silica matrix as filler；It is described molten
Liquid A is acetonitrile, and the solution B is phosphoric acid water；The ingredient includes glycycoumarin, isoliquiritigenin, celery sugar liquiritin, shaddock ped rue
One of fragrant glycosides, liquiritin, nobiletin are a variety of.
Further, the mass concentration of the phosphoric acid water is 0.05%-0.15%.
As a preference, the mass concentration of the phosphoric acid water is 0.05%.
Further, it is 0.5-1.5ml/min that the mobile phase, which carries out the flow velocity of gradient elution,.
As a preference, the flow velocity that the mobile phase carries out gradient elution is 1.0ml/min.
Further, detector wavelength 250-280nm.
As a preference, detector wavelength is 280nm.
Further, detector column temperature is 25-30 DEG C.
As a preference, detector column temperature is 25 DEG C.
Further, condition of gradient elution are as follows:
The percent by volume of 0-10min, mobile phase A and Mobile phase B is 8-18:92-82；
The percent by volume of 10-15min, mobile phase A and Mobile phase B is 18-19:82-81；
The percent by volume of 15-17min, mobile phase A and Mobile phase B is 19:81；
The percent by volume of 17-23min, mobile phase A and Mobile phase B is 19-20:81-80；
The percent by volume of 23-27min, mobile phase A and Mobile phase B is 20:80；
The percent by volume of 27-30min, mobile phase A and Mobile phase B is 20-21:80-79；
The percent by volume of 30-35min, mobile phase A and Mobile phase B is 21:79；
The percent by volume of 35-38min, mobile phase A and Mobile phase B is 21-22:79-78；
The percent by volume of 38-41min, mobile phase A and Mobile phase B is 22-23:78-77；
The percent by volume of 41-45min, mobile phase A and Mobile phase B is 23-26:77-74；
The percent by volume of 45-51min, mobile phase A and Mobile phase B is 26-32:74-68；
The percent by volume of 51-54min, mobile phase A and Mobile phase B is 32-33:68-67；
The percent by volume of 54-62min, mobile phase A and Mobile phase B is 33-55:67-45；
The percent by volume of 62-72min, mobile phase A and Mobile phase B is 55-74:45-26；
The percent by volume of 72-75min, mobile phase A and Mobile phase B is 74-75:26-25；
The percent by volume of 75-77min, mobile phase A and Mobile phase B is 75:25；
The percent by volume of 77-80min, mobile phase A and Mobile phase B is 75-100:25-0；
The percent by volume of 80-83min, mobile phase A and Mobile phase B is 100:0；
The percent by volume of 83-85min, mobile phase A and Mobile phase B is 100-8:0-92.
Gradient elution is the professional term of a field of pharmaceutical preparations, is referred in the same analytical cycle, by certain journey
The concentration proportioning that degree constantly changes mobile phase carrys out separate substance.In HPLC analysis, the concrete composition and its gradient of mobile phase become
Change is the important parameter for realizing the separation analysis of multi-component complex sample.
The two of the object of the invention are to provide Multiple components content in a kind of HPLC method separation determination ageratum oral liquid
Specific method.
According to the method for Multiple components content in a kind of above-mentioned HPLC method separation determination ageratum oral liquid, step is such as
Under:
1) it prepares reference substance solution: weighing suitable glycycoumarin, isoliquiritigenin, celery sugar liquiritin, shaddock ped rue respectively
Fragrant glycosides, liquiritin, nobiletin add methanol solution dissolution that reference substance solution is prepared；
2) it prepares sample solution: weighing suitable ageratum oral liquid, diluted with methanol solution and sample solution is made；
As a preference, taking ageratum oral liquid 5 of every 10mL to mix, 2mL recycling design is taken, is weighed
162.3mg, with methanol dilution to 10mL to get；
3) the sample solution injection high performance liquid chromatograph of the reference substance solution and step 2) that take step 1) respectively is divided
Analysis records chromatogram, and each peak separating degree should be greater than 1.5, calculates glycycoumarin, different Radix Glycyrrhizae in sample solution using external standard method
Element, celery sugar liquiritin, narirutin, liquiritin, nobiletin content.
The three of the object of the invention are to provide a kind of reagent of Multiple components content in separation determination ageratum oral liquid
Composition.
It is a kind of for be separated by solid-liquid separation measurement ageratum oral liquid in Multiple components content reagent composition, the ingredient
Including one of glycycoumarin, isoliquiritigenin, celery sugar liquiritin, narirutin, liquiritin, nobiletin or a variety of；Institute
Reagent composition is stated using silica gel as stationary phase, using acetonitrile as reagent A, using phosphoric acid water as reagent B；The phosphoric acid water
Mass concentration is 0.05%-0.15%.
As a preference, the mass concentration of the phosphoric acid water is 0.05%.
The three of the object of the invention are to provide a kind of separation determination glycycoumarin, isoliquiritigenin, celery sugar Radix Glycyrrhizae simultaneously
The HPLC method of this component content in 6 of glycosides, narirutin, liquiritin, nobiletin.
A kind of separation determination glycycoumarin, isoliquiritigenin, celery sugar liquiritin, narirutin, liquiritin and river simultaneously
The HPLC method of skin glycosides content, the chromatographic column that the HPLC method uses are using silica matrix as filler, with solution A and solution B
It is mixed in a certain ratio and is eluted for mobile phase；The solution A is acetonitrile, and the solution B is phosphoric acid water.
Further, condition of gradient elution are as follows:
The percent by volume of 0-10min, mobile phase A and Mobile phase B is 8-18:92-82；
The percent by volume of 10-15min, mobile phase A and Mobile phase B is 18-19:82-81；
The percent by volume of 15-17min, mobile phase A and Mobile phase B is 19:81；
The percent by volume of 17-23min, mobile phase A and Mobile phase B is 19-20:81-80；
The percent by volume of 23-27min, mobile phase A and Mobile phase B is 20:80；
The percent by volume of 27-30min, mobile phase A and Mobile phase B is 20-21:80-79；
The percent by volume of 30-35min, mobile phase A and Mobile phase B is 21:79；
The percent by volume of 35-38min, mobile phase A and Mobile phase B is 21-22:79-78；
The percent by volume of 38-41min, mobile phase A and Mobile phase B is 22-23:78-77；
The percent by volume of 41-45min, mobile phase A and Mobile phase B is 23-26:77-74；
The percent by volume of 45-51min, mobile phase A and Mobile phase B is 26-32:74-68；
The percent by volume of 51-54min, mobile phase A and Mobile phase B is 32-33:68-67；
The percent by volume of 54-62min, mobile phase A and Mobile phase B is 33-55:67-45；
The percent by volume of 62-72min, mobile phase A and Mobile phase B is 55-74:45-26；
The percent by volume of 72-75min, mobile phase A and Mobile phase B is 74-75:26-25；
The percent by volume of 75-77min, mobile phase A and Mobile phase B is 75:25；
The percent by volume of 77-80min, mobile phase A and Mobile phase B is 75-100:25-0；
The percent by volume of 80-83min, mobile phase A and Mobile phase B is 100:0；
The percent by volume of 83-85min, mobile phase A and Mobile phase B is 100-8:0-92.
The beneficial effects of the present invention are:
1) the present invention provides a kind of methods of Multiple components content in HPLC method separation determination ageratum oral liquid, should
Method is able to achieve efficiently separating for glycycoumarin, isoliquiritigenin, celery sugar liquiritin, narirutin, liquiritin and nobiletin.
2) this method is simple, sensitive, accuracy is high, can make up the prior art and be not enough to illustrate in ageratum oral liquid
The defect of component content effectively ensures the quality of ageratum oral liquid.
Detailed description of the invention
Fig. 1 HPLC analyzes map.
Specific embodiment
Hereinafter reference will be made to the drawings, and the preferred embodiment of the present invention is described in detail.Illustrated embodiment is in order to more preferable
Ground is illustrated the contents of the present invention, but is not that the contents of the present invention are only limitted to illustrated embodiment.So being familiar with this field
Technical staff nonessential modifications and adaptations are carried out to embodiment according to foregoing invention content, still fall within protection of the invention
Range.
1. laboratory apparatus
SartoriusBP211D type electronic balance (German Sai Tuolisi company)；(Sichuan is excellent general super for Hyperpure water manufacturing systems
Pure Science and Technology Ltd.)；Sai Mo flies UltiMate 3000 (match is silent to fly).
2. experimental material
Tai Ji ageratum oral liquid (Taiji Group Chongqing Fuling Pharmaceutical Factory Co., Ltd., lot number 17080319).
The preferred Tai Ji ageratum oral liquid of the present embodiment, but the present invention is not limited to the ageratum mouths of Tai Ji pharmaceutical factory
Take liquid.
Glycycoumarin, isoliquiritigenin, celery sugar liquiritin, narirutin, liquiritin, nobiletin；Methanol, acetonitrile；Two
Secondary distilled water.
Embodiment 1
1. reference substance stock solution
Precision weighs glycycoumarin, isoliquiritigenin, celery sugar liquiritin, narirutin, liquiritin, appropriate nobiletin,
0.07450,0.50002,0.97600,0.50010,0.50000,0.62700mg/ml is respectively prepared after additive color spectrum methanol dissolution
Reference substance stock solution, be stored in spare in 4 DEG C of refrigerators.
2. standard curve
Precision draws the glycycoumarin reference substance stock solution 1) under item, successively dilute every 1mL containing 0.0075,
0.0037,0.0019,0.0009,0.0006,0.0005mg, obtain the reference substance solution of 6 groups of various concentrations, number 1~6；It is accurate
Draw the isoliquiritigenin reference substance stock solution 1) under item, successively dilute every 1mL containing 0.0250,0.0125,0.0063,
0.0031,0.0016,0.0008mg, obtain the reference substance solution of 6 groups of various concentrations, number 1~6；Precision draws the celery under 1) item
Sugared liquiritin reference substance stock solution, successively dilute every 1mL containing 0.9760,0.0976,0.0488,0.0244,0.0122,
0.0061mg obtains the reference substance solution of 6 groups of various concentrations, number 1~6；Precision draws the narirutin reference substance under 1) item
Stock solution, successively dilute every 1mL containing 0.2500,0.0500,0.0250,0.0125,0.0063,0.0016mg, obtain 6 groups of differences
The reference substance solution of concentration, number 1~6；Precision draws the liquiritin reference substance stock solution under 1) item, successively dilutes to obtain every 1mL
Containing 0.2500,0.1250,0.0625,0.0313,0.0156,0.0078mg, the reference substance solution of 6 groups of various concentrations, number 1 are obtained
~6；Precision draws the nobiletin reference substance stock solution 1) under item, successively dilute every 1mL containing 0.0627,0.0063,0.0031,
0.0016,0.0007,0.0004mL, obtain the reference substance solution of 6 groups of various concentrations, number 1~6；It measures according to the following steps.With right
According to the concentration (mgmL of product-1) it is abscissa (X), peak area (mAU) is ordinate (Y), draws standard curve, obtains recurrence side
Journey and related coefficient.
2.1 chromatographic conditions and system suitability Kromasil EternityXT-5-C18 column (4.6 × 250mm, 5 μm), stream
Dynamic phase acetonitrile (A) -0.05% phosphoric acid water (B).Gradient elution: 0~10min, 8%~18%A；10~15min, 18%~19%
A；15~17min, 19%~19%A；17~23min, 19%~20%A；23~27min, 20%~20%A；27~
30min, 20%~21%A；30~35min, 21%~21%A；35~38min, 21%~22%A；38~41min, 22%
~23%A；41~45min, 23%~26%A；45~51min, 26%~32A；51~54min, 32%~33%A；54~
62min, 33%~55%A；62~72min, 55%~74%A；72~75min, 74%~75%A；75~77min, 75%
~75%A；77~80min, 75%~100%A；80~83min, 100%~100%A；83~85min, 100%~8%A.
Flow velocity 1mL/min；Detection wavelength 280nm；25 DEG C of column temperature；10 μ L of sample volume.Each peak separating degree is all larger than 1.5.
2.2 equation of linear regression
The equation of linear regression of 16 kinds of ingredients of table
Embodiment 2
1. precision
6 kinds of reference substance stock solutions of accurate measurement are appropriate respectively, obtain every 1mL with methanol dilution and contain 0.002,0.050,0.005,
The mixed solution of the above-mentioned 6 kinds of ingredients of 0.010,0.050 and 0.003mg.10 μ L of mixed solution is taken, by embodiment 1 " 2.1 " Xiang Jinhang
Measurement.Continuous sample introduction 6 times, record peak area.As a result glycycoumarin, isoliquiritigenin, celery sugar liquiritin, narirutin, sweet
Careless glycosides, nobiletin peak area RSD value be respectively 1.06%, 0.17%, 1.43%, 1.24%, 0.23%, 0.15%, 6 kinds at
The RSD value of swarming area is respectively less than 3%, shows that instrument precision is good.
2. repeatability
Take 1 is 17080319 sample preparation test solution in batches number, prepares sample by method provided by the invention, then
Every 1mL above-mentioned 6 kinds of ingredients Han 0.0020,0.0500,0.0050,0.0100,0.0500 and 0.0030mg are obtained with methanol dilution
Test solution is mixed, is measured by embodiment 1 " 2.1 " item.As a result glycycoumarin, isoliquiritigenin, celery sugar liquiritin, shaddock ped rue
Fragrant glycosides, liquiritin, nobiletin peak area RSD value be respectively 2.88%, 0.53%, 0.56%, 0.40%, 0.36%,
1.81%, the RSD value of 6 kinds of Component peak areas is respectively less than 3%, shows each ingredient weight in 48h in Tai Ji ageratum oral liquid
Renaturation is good.
3. stability
Take 1 is a 17080319 sample preparation test solution in batches number, respectively at the 0th, 12,24,36 and 48h, by real
It applies and is measured under example 1 " 2.1 " item.As a result glycycoumarin, isoliquiritigenin, celery sugar liquiritin, narirutin, liquiritin,
The RSD value of nobiletin peak area is respectively 1.92%, 0.09%, 0.51%, 1.43%, 0.85%, 0.45%, and 6 kinds at swarming
The RSD value of area is respectively less than 3%, shows that each ingredient is good in 48h internal stability in Tai Ji ageratum oral liquid.
4. sample recovery rate
Taking lot number is 17080319 sample, and precision weighs 6 parts, is separately added into the reference substance solution of sample equivalent, by this
The method that invention provides prepares sample, again with methanol dilute every 1mL containing 0.0019,0.0500,0.0049,0.0100,
The mixing test solution of the above-mentioned 6 kinds of ingredients of 0.0500 and 0.0031mg is measured by embodiment 1 " 2.1 " item, records peak area,
Calculate mean sample recovery rate.As a result glycycoumarin, isoliquiritigenin, celery sugar liquiritin, narirutin, liquiritin, river skin
Glycosides mean sample recovery rate difference 95.70%, 97.79%, 99.74%, 103.15%, 100.71%, 103.72%, RSD value
Respectively 1.04%, 0.50%, 0.56%, 0.19%, 1.54%, 0.23%.
Embodiment 3
Sample measurement
1 batch of sample is handled in the present inventive method, by being measured under embodiment 1 " 2.1 " item, is calculated using external standard method sweet
Hay-scented legumin, isoliquiritigenin, celery sugar liquiritin, narirutin, liquiritin, nobiletin content, be as a result respectively
0.007%, 0.251%, 0.221%, 0.279%, 0.540% and 0.009%.
Table 2 10 batches of Tai Ji ageratum oral liquid samples, 6 kinds of component contents
Finally, it is stated that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although referring to compared with
Good embodiment describes the invention in detail, those skilled in the art should understand that, it can be to skill of the invention
Art scheme is modified or replaced equivalently, and without departing from the objective and range of technical solution of the present invention, should all be covered at this
In the scope of the claims of invention.
Claims (10)
1. a kind of method of Multiple components content in HPLC method separation determination ageratum oral liquid, which is characterized in that described
The chromatographic column that HPLC method uses is to be mixed in a certain ratio using silica matrix as filler with solution A and solution B as mobile phase progress
Elution；The solution A is acetonitrile, and the solution B is phosphoric acid water；The ingredient includes that glycycoumarin, isoliquiritigenin, celery sugar are sweet
One of careless glycosides, narirutin, liquiritin, nobiletin are a variety of.
2. the side of Multiple components content in a kind of HPLC method separation determination ageratum oral liquid according to claim 1
Method, which is characterized in that the mass concentration of the phosphoric acid water is 0.05%-0.15%.
3. the side of Multiple components content in a kind of HPLC method separation determination ageratum oral liquid according to claim 1
Method, which is characterized in that the flow velocity that the mobile phase carries out gradient elution is 0.5-1.5ml/min.
4. the side of Multiple components content in a kind of HPLC method separation determination ageratum oral liquid according to claim 1
Method, which is characterized in that detector wavelength 250-280nm.
5. the side of Multiple components content in a kind of HPLC method separation determination ageratum oral liquid according to claim 1
Method, which is characterized in that detector column temperature is 25-30 DEG C.
6. the side of Multiple components content in a kind of HPLC method separation determination ageratum oral liquid according to claim 1
Method, which is characterized in that condition of gradient elution are as follows:
The percent by volume of 0-10min, mobile phase A and Mobile phase B is 8-18:92-82；
The percent by volume of 10-15min, mobile phase A and Mobile phase B is 18-19:82-81；
The percent by volume of 15-17min, mobile phase A and Mobile phase B is 19:81；
The percent by volume of 17-23min, mobile phase A and Mobile phase B is 19-20:81-80；
The percent by volume of 23-27min, mobile phase A and Mobile phase B is 20:80；
The percent by volume of 27-30min, mobile phase A and Mobile phase B is 20-21:80-79；
The percent by volume of 30-35min, mobile phase A and Mobile phase B is 21:79；
The percent by volume of 35-38min, mobile phase A and Mobile phase B is 21-22:79-78；
The percent by volume of 38-41min, mobile phase A and Mobile phase B is 22-23:78-77；
The percent by volume of 41-45min, mobile phase A and Mobile phase B is 23-26:77-74；
The percent by volume of 45-51min, mobile phase A and Mobile phase B is 26-32:74-68；
The percent by volume of 51-54min, mobile phase A and Mobile phase B is 32-33:68-67；
The percent by volume of 54-62min, mobile phase A and Mobile phase B is 33-55:67-45；
The percent by volume of 62-72min, mobile phase A and Mobile phase B is 55-74:45-26；
The percent by volume of 72-75min, mobile phase A and Mobile phase B is 74-75:26-25；
The percent by volume of 75-77min, mobile phase A and Mobile phase B is 75:25；
The percent by volume of 77-80min, mobile phase A and Mobile phase B is 75-100:25-0；
The percent by volume of 80-83min, mobile phase A and Mobile phase B is 100:0；
The percent by volume of 83-85min, mobile phase A and Mobile phase B is 100-8:0-92.
7. Multiple components contain in a kind of HPLC method separation determination ageratum oral liquid according to claim 1-6
The method of amount, which is characterized in that steps are as follows:
1) prepare reference substance solution: weigh respectively suitable glycycoumarin, isoliquiritigenin, celery sugar liquiritin, narirutin,
Liquiritin, nobiletin add methanol solution dissolution that reference substance solution is prepared；
2) it prepares sample solution: weighing suitable ageratum oral liquid, diluted with methanol solution and sample solution is made；
3) the sample solution injection high performance liquid chromatograph of the reference substance solution and step 2) that take step 1) respectively is analyzed, and is remembered
Chromatogram is recorded, calculates glycycoumarin, isoliquiritigenin, celery sugar liquiritin, narirutin, Radix Glycyrrhizae in sample solution with external standard method
Glycosides, nobiletin content.
8. a kind of for being separated by solid-liquid separation the reagent composition of Multiple components content in measurement ageratum oral liquid, feature exists
In, the ingredient include glycycoumarin, isoliquiritigenin, celery sugar liquiritin, narirutin, liquiritin, one in nobiletin
Kind is a variety of；The reagent composition uses reverse phase silica gel as stationary phase, using acetonitrile as reagent A, using phosphoric acid water as examination
Agent B；The mass concentration of the phosphoric acid water is 0.05%-0.15%.
9. a kind of separation determination glycycoumarin, isoliquiritigenin, celery sugar liquiritin, narirutin, liquiritin and river skin simultaneously
The HPLC method of glycosides content, which is characterized in that the chromatographic column that the HPLC method uses is using silica matrix as filler, with solution
A and solution B are mixed in a certain ratio to be eluted for mobile phase；The solution A is acetonitrile, and the solution B is phosphoric acid water.
10. HPLC method according to claim 9, which is characterized in that condition of gradient elution are as follows:
The percent by volume of 0-10min, mobile phase A and Mobile phase B is 8-18:92-82；
The percent by volume of 10-15min, mobile phase A and Mobile phase B is 18-19:82-81；
The percent by volume of 15-17min, mobile phase A and Mobile phase B is 19:81；
The percent by volume of 17-23min, mobile phase A and Mobile phase B is 19-20:81-80；
The percent by volume of 23-27min, mobile phase A and Mobile phase B is 20:80；
The percent by volume of 27-30min, mobile phase A and Mobile phase B is 20-21:80-79；
The percent by volume of 30-35min, mobile phase A and Mobile phase B is 21:79；
The percent by volume of 35-38min, mobile phase A and Mobile phase B is 21-22:79-78；
The percent by volume of 38-41min, mobile phase A and Mobile phase B is 22-23:78-77；
The percent by volume of 41-45min, mobile phase A and Mobile phase B is 23-26:77-74；
The percent by volume of 45-51min, mobile phase A and Mobile phase B is 26-32:74-68；
The percent by volume of 51-54min, mobile phase A and Mobile phase B is 32-33:68-67；
The percent by volume of 54-62min, mobile phase A and Mobile phase B is 33-55:67-45；
The percent by volume of 62-72min, mobile phase A and Mobile phase B is 55-74:45-26；
The percent by volume of 72-75min, mobile phase A and Mobile phase B is 74-75:26-25；
The percent by volume of 75-77min, mobile phase A and Mobile phase B is 75:25；
The percent by volume of 77-80min, mobile phase A and Mobile phase B is 75-100:25-0；
The percent by volume of 80-83min, mobile phase A and Mobile phase B is 100:0；
The percent by volume of 83-85min, mobile phase A and Mobile phase B is 100-8:0-92.
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| CN114200038A (en) * | 2021-11-23 | 2022-03-18 | 太极集团重庆涪陵制药厂有限公司 | Method for detecting compound content in wrinkled gianthyssop herb zhengqi oral liquid by liquid chromatography-mass spectrometry |
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| CN114200038A (en) * | 2021-11-23 | 2022-03-18 | 太极集团重庆涪陵制药厂有限公司 | Method for detecting compound content in wrinkled gianthyssop herb zhengqi oral liquid by liquid chromatography-mass spectrometry |
| CN114200038B (en) * | 2021-11-23 | 2023-08-29 | 太极集团重庆涪陵制药厂有限公司 | Method for detecting compound content in agastache rugosa healthy qi oral liquid by liquid chromatography-mass spectrometry |
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