CN106706825A - Method used for measuring content of tetrahydropalmatine in rhizoma cyperi-tangerine leaf capsule used for treating breast hyperplasia - Google Patents
Method used for measuring content of tetrahydropalmatine in rhizoma cyperi-tangerine leaf capsule used for treating breast hyperplasia Download PDFInfo
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Abstract
The invention relates to a method used for measuring the content of tetrahydropalmatine in rhizoma cyperi-tangerine leaf capsule used for treating breast hyperplasia. The method comprises following steps: 1, a reference substance solution is prepared; 2, a sample solution to be tested is prepared; 3, the reference substance solution and the sample solution are injected into a high performance liquid chromatograph so as to obtain chromatograms; and 4, the content of tetrahydropalmatine in the sample to be tested is calculated based on the chromatograms.
Description
Technical field：
The present invention relates to a kind of detection method of active ingredient in medicine, prolong during more particularly to a kind of fragrant tangerine breast addiction is peaceful
The content assaying method of Hu Suo Yisu.
Background technology:
Fragrant tangerine breast addiction Yiganning capsule is that a kind of dispersing stagnated hepatoqi is relieved pain, blood circulation promoting and dispersing pathogen accumulation menstruation regulating, and for stagnation of QI due to depression of the liver, phlegm coagulates
The Chinese medicine preparation of the cyclomastopathy caused by blood stasis, is still in conceptual phase at present, withered by rhizoma cyperi, tangerine leaf, summer
The Chinese medicines such as grass, the red sage root, the rhizoma bolbostemmae, corydalis tuber, China rose are prepared from.Wherein with rhizoma cyperi as monarch drug in a prescription, tangerine
Leaf is ministerial drug.
The preparation method of fragrant tangerine breast addiction Yiganning capsule is：Take tangerine leaf, selfheal, China rose, plus the decocting of 12 times of amounts
Boil 3 times, 1 hour every time, collecting decoction, filtration, filtrate decompression was concentrated into relative density 1.08-1.10 (60 DEG C)
Clear cream, plus ethanol makes alcohol content up to 70%, stands overnight, and takes supernatant, is concentrated under reduced pressure into relative density
The thick paste of 1.28-1.30 (60 DEG C), drying under reduced pressure is standby；Separately take rhizoma cyperi, the red sage root, the rhizoma bolbostemmae, corydalis tuber etc.
Four tastes add 70% ethanol to extract 3 times, for the first time 7 times of amounts, second and third each 6 times of amount, 1.5 hours every time,
Merge extract solution, filtration, filtrate decompression is concentrated into the thick paste of relative density 1.28-1.30 (60 DEG C), drying under reduced pressure,
Merge with above-mentioned water extract-alcohol precipitation dry cream, be ground into fine powder, by above-mentioned dried cream powder and appropriate amount of starch, microcrystalline cellulose
Mix, granulation adds magnesium stearate, superfine silica gel powder, mixes, fill capsule, it is aluminum-plastic packaged, obtain final product.
Tetrahydropalmatine is the main component of corydalis tuber, be index in the breast addiction Yiganning capsule quality control of fragrant tangerine into
Point.The content assaying method of tetrahydropalmatine is (to be used using the phosphoric acid of acetonitrile -0.1% in perfume tangerine breast addiction Yiganning capsule at present
Triethylamine adjusts pH to 7.0) (40:60) it is mobile phase, 30 DEG C of column temperature, however, being existed very in current method
Many defects, for example：The separating degree of target component is more sensitive to pH value, and preparation mobile phase repeatability is poor,
Baseline is seriously drifted about, deformed after sample continuous sample introduction, easily stifled post after continuous sample introduction spininess, and post pressure is raised etc..
The content of the invention:
In order to solve the above problems, the present invention is right on the basis of original Content determination of dl-tetrahydropalmatine assay method
Content determination of dl-tetrahydropalmatine assay method is optimized, and the Content determination of dl-tetrahydropalmatine assay method after optimization is specific such as
Under：
The content assaying method of tetrahydropalmatine, comprises the following steps during a kind of fragrant tangerine breast addiction is peaceful：
Step 1, the preparation of reference substance solution,
Step 2, the preparation of need testing solution,
Step 3, by reference substance solution and need testing solution injection high performance liquid chromatograph, obtains chromatogram,
Step 4, the content of tetrahydropalmatine in test sample is calculated according to chromatogram,
Wherein chromatographic condition is as follows：
Wherein number of theoretical plate is calculated by tetrahydropalmatine peak and should be not less than 3000.Chromatographic column uses octadecylsilane
Bonded silica gel is filler, and mobile phase is the acetonitrile-triethylamine aqueous solution, the volume ratio of triethylamine in its reclaimed water phase
It is 0.01~0.03%, Detection wavelength is 265-295nm, 25-45 DEG C of column temperature.Detection wavelength is 280nm.Post
35 DEG C of temperature.Gradient elution program is as follows：
The wherein preparation of reference substance solution described in step 1, method is as follows：
Tetrahydropalmatine reference substance plus methyl alcohol are taken, the solution of every 1ml μ containing 5-20 g is made.Preferably, method
It is as follows：Weigh tetrahydropalmatine reference substance in right amount, plus methyl alcohol is made solution of every 1ml containing 10 μ g, obtains final product.
The preparation of need testing solution wherein described in step 2, method is as follows：Detection sample is finely ground, takes 0.1-1g
Plus Diluted Alcohol 5-20ml, ultrasonically treated more than 15min, let cool, plus filtered after Diluted Alcohol dilution, take continuous filter
Liquid, obtains final product.Preferably, method is as follows：This product content is taken, it is finely ground, about 0.3g is taken, it is accurately weighed, put
In 10ml measuring bottles, plus Diluted Alcohol about 8ml, ultrasonically treated 15 minutes (120W, 40KHz) lets cool, plus dilute
Ethanol is diluted to scale, shakes up, filtration, takes subsequent filtrate, obtains final product.
The method of wherein step 3 is as follows：Reference substance solution 5-20 μ l, need testing solution 5-20 μ l are taken respectively,
Injection liquid chromatograph, obtains chromatogram, and the content of tetrahydropalmatine is calculated with external standard two-point method logarithmic equation.
Preferred method is as follows：It is accurate respectively to draw reference substance solution and each 10 μ l of need testing solution, inject liquid chromatogram
Instrument, determines, and obtains final product.
The chromatographic condition of this method is obtained by screening：
1st, the selection of wavelength is determined
UV scanning is carried out through to tetrahydropalmatine reference substance solution, there is maximum absorption band at 282nm, joined
Former method is examined, 280nm is still selected as Detection wavelength.
2nd, the selection of mobile phase
In former method, using the phosphoric acid of acetonitrile -0.1% (adjusting pH to 7.0 with triethylamine), the two ratio is mobile phase
40:60, but the separating degree of target component is more sensitive to pH value, preparation mobile phase repeatability is poor, separating degree
It is bad, there is acromion.See Fig. 1.
In order to solve the problem, according to the property of tetrahydropalmatine, to avoid peak shape from trailing, selection alkalescence flowing
Phase condition, contrasts through investigating, and used as water phase, peak shape is good, does not trail for 0.02% triethylamine water of selection, not before
Prolong, when triethylamine concentration is respectively 0.01%, 0.02%, 0.03%, peak shape is good, this mobile phase prepares letter
It is single, it is easy to operate, therefore the selection triethylamine of acetonitrile -0.02% water is mobile phase.Chromatogram is shown in Fig. 2
3 solution manufacturing methods
With original method, former method is to Extraction solvent, extraction time and pure for the compound method of reference substance and test sample
Change method by investigating, have selected optimal parameter, therefore new method selection is prepared with former method identical solution
Method.
4 methodological studies
4.1 specificities are tested
Respectively precision measure blank solvent, lack corydalis tuber feminine gender solution, tetrahydropalmatine reference substance solution, for examination
Each 10 μ l of product solution, inject liquid chromatograph, record liquid chromatogram.From liquid chromatogram, herein
Tetrahydropalmatine and other components can reach baseline separation under chromatographic condition, lack corydalis tuber negative sample with prolong recklessly
Occur without absworption peak on Suo Yisu reference substances relevant position, number of theoretical plate is calculated by tetrahydropalmatine peak and is not less than
3000.Result is shown in Fig. 3, Fig. 4, Fig. 5, Fig. 6.
4.2 instrument precisions are tested
It is 2.39 μ g/ml, 11.97 μ g/ml, the reference substance solution of 35.90 μ g/ml, precision to take concentration respectively
The μ l of reference substance solution 10 are drawn, METHOD FOR CONTINUOUS DETERMINATION 6 times the results are shown in Table 2.
The Precision test result of table 2
Result of the test shows：Under senior middle school's low concentration, instrument precision is good.
4.3 is linear
Precision weighs tetrahydropalmatine reference substance 11.98mg, and in putting 100ml measuring bottles, plus methyl alcohol makes dissolving and dilute
Release to scale, shake up, the reference substance solution (mother liquor) of 119.8 μ g/ml is obtained.Mother liquor is done into following dilution：
1ml→50ml；1ml→25ml；2ml→25ml；1ml→10ml；3ml→25ml；3ml→10ml
It is accurate respectively to draw above-mentioned each 10 μ l of solution, liquid chromatograph is injected, determine.It is vertical with peak area (A)
Coordinate (Y), with its sample size (μ g) as abscissa (X), linear regression is carried out by least square method, the results are shown in Table 3
And Fig. 7.
The investigation of the linear relationship of table 3
Result of the test shows：In 0.0239~0.359 μ g ranges, it enters tetrahydropalmatine reference substance sample size
Sample amount (μ g) is in good linear relationship with peak area.
4.4 replica tests
This product (lot number 20131004) content taken under content uniformity is finely ground, weighs 6 parts, every part of about 0.3g,
It is accurately weighed respectively, in putting 10ml volumetric flasks, plus Diluted Alcohol about 8ml, ultrasonically treated 15 minutes, let cool,
Plus Diluted Alcohol is diluted to scale, shake up, filter, take subsequent filtrate, obtain final product.It is accurate respectively to draw reference substance solution
10 μ l each with need testing solution, injects liquid chromatograph, determines, and the results are shown in Table 4.
The replica test result of table 4
Result of the test shows：6 parts of coefficient of variation RSD=1.90% of sample size are measured, shows the weight of method
Renaturation is good.
4.5 Intermediate precisions
Instrument is changed, this product (lot number 20131004) content taken under content uniformity is finely ground, weighs 6 parts,
Every part of about 0.3g, it is accurately weighed respectively, in putting 10ml volumetric flasks, plus Diluted Alcohol about 8ml, ultrasonically treated 15
Minute, let cool, plus Diluted Alcohol is diluted to scale, shakes up, filtration, takes subsequent filtrate, obtains final product.It is accurate respectively to inhale
Reference substance solution and each 10 μ l of need testing solution are taken, liquid chromatograph is injected, determined, the results are shown in Table 5.
The Intermediate precision result of the test of table 5
Result of the test shows：6 parts of coefficient of variation RSD=0.89% of sample size are measured, separately by intermediate precision
Degree 6 measurement result joint accounts of 6 measurement results and replica test, average value is 0.0221mg/g,
RSD=4.17%, shows that the reappearance of method is good.
4.6 recovery tests
(lot number 20131004, content is based on the average value of replica test to take the test sample of known content
0.023mg/g) 6 parts, every part of about 0.15g is accurately weighed, puts in 10ml volumetric flasks, and accurate addition is dense respectively
The tetrahydropalmatine reference substance 1ml for 35.90 μ g/m is spent, the preparation method according to need testing solution prepares 6 parts
Need testing solution, it is accurate respectively to draw reference substance solution and each 10 μ l of need testing solution, liquid chromatograph is injected,
Determine, the results are shown in Table 7.
The recovery test result of table 6
Result of the test shows：The method rate of recovery is good.
4.7 serviceability tests
To investigate the durability of the method, we are respectively by temperature, Detection wavelength, flow velocity, chromatographic column, three second
The factor such as amine concentration and proportion of mobile phase fluctuates in a small range, assay is carried out with same sample, with each time
The RSD of size of experiment measurement result is investigated for inspection target to it.Result and its analysis be shown in Table 7 respectively,
Table 8.
The durability of table 7 investigates result
By above experimental result, its reductive analysis is obtained following analysis result by us：
The durability of table 8 investigates interpretation of result
Upper table and each chromatogram result show that each typical variable of the method is separated when a small range changes
Degree is unaffected, and because content is relatively low, therefore each factor RSD values in change are larger, except column temperature, other
Variable RSD is respectively less than 5%, and in tolerance interval, when column temperature changes upper and lower 5 DEG C, RSD is 8.44%,
Show that column temperature influences larger to measurement result, be should be noted that in continuous mode.Column temperature be set to 35 DEG C come from compared with
Under high-temperature, sample component absorption is smaller in chromatographic column, more is rinsed, when being unlikely to use one section
Between after chromatographic column block, pressure drastically raises.
4.8 methods are contrasted
This product (lot number 20131004) content taken under content uniformity is finely ground, weighs 2 parts, every part of about 0.3g,
Assay is carried out with former method and new method respectively, 9 are the results are shown in Table.
The method comparing result of table 9
Result of the test shows：Two methods are consistent in measurement result.
5. summarize
By checking, new method can be used for the measure of Content determination of dl-tetrahydropalmatine in fragrant tangerine breast addiction Yiganning capsule, resistance to
It is better than former method with property, convenient operation.And separating degree is to pH sensitive, pH in overcoming former method
Value varies slightly the problem that separating degree declines, and baseline drift, deformation and easily stifled post, post after continuous sample introduction
The problems such as pressure is easily raised.
Brief description of the drawings：
Fig. 1 original method chromatograms
Fig. 2 the inventive method chromatograms
Fig. 3 blank solvents
It is negative that Fig. 4 lacks corydalis tuber
Fig. 5 tetrahydropalmatine contrast solutions
Fig. 6 contrast solutions
Fig. 7 tetrahydropalmatines method containing survey is linear
Specific embodiment：
The present invention is further illustrated by the following examples.
Embodiment 1
(1) instrument：Waters e2695 high performance liquid chromatographs；Waters Empower Pro work stations, Waters
2998 type UV-detectors.
(2) reagent and reagent
Tetrahydropalmatine reference substance：There is provided by National Institute for Food and Drugs Control, for assay, lot number：
110726-201414.Methyl alcohol, acetonitrile are chromatographically pure, and ethanol, phosphoric acid, triethylamine are pure for analysis, and water is new
Fresh two pure water.
(3) chromatographic condition：It is filler with octadecylsilane chemically bonded silica；The triethylamine water of acetonitrile -0.02%
It is mobile phase, gradient elution such as table 1；Detection wavelength is 280nm, 35 DEG C of column temperature.Number of theoretical plate by prolong recklessly
Suo Yisu peaks are calculated and should be not less than 3000.
Table 1：Eluent gradient
Embodiment 2
(1) Waters e2695 high performance liquid chromatographs；Waters Empower Pro work stations, Waters 2489
Type UV-detector.
(2) reagent and reagent
Tetrahydropalmatine reference substance：There is provided by National Institute for Food and Drugs Control, for assay, lot number：
110726-201414.Methyl alcohol, acetonitrile are chromatographically pure, and ethanol, phosphoric acid, triethylamine are pure for analysis, and water is new
Fresh two pure water.
(3) chromatographic condition：It is filler with octadecylsilane chemically bonded silica；The triethylamine water of acetonitrile -0.01%
It is mobile phase, gradient elution such as table 1；Detection wavelength is 265nm, 25 DEG C of column temperature.Number of theoretical plate presses corydalis tuber
B prime peak is calculated and should be not less than 3000.
Table 1：Eluent gradient
Embodiment 3
(1) Waters e2695 high performance liquid chromatographs；Waters Empower Pro work stations, Waters 2489
Type UV-detector.
(2) reagent and reagent
Tetrahydropalmatine reference substance：There is provided by National Institute for Food and Drugs Control, for assay, lot number：
110726-201414.Methyl alcohol, acetonitrile are chromatographically pure, and ethanol, phosphoric acid, triethylamine are pure for analysis, and water is new
Fresh two pure water.
(3) chromatographic condition：It is filler with octadecylsilane chemically bonded silica；The triethylamine water of acetonitrile -0.03%
It is mobile phase, gradient elution such as table 1；Detection wavelength is 295nm, 45 DEG C of column temperature.Number of theoretical plate by prolong recklessly
Suo Yisu peaks are calculated and should be not less than 3000.
Table 1：Eluent gradient
Claims (10)
1. the content assaying method of tetrahydropalmatine, comprises the following steps during a kind of fragrant tangerine breast addiction is peaceful：
Step 1, the preparation of reference substance solution,
Step 2, the preparation of need testing solution,
Step 3, by reference substance solution and need testing solution injection high performance liquid chromatograph, obtains chromatogram,
Step 4, the content of tetrahydropalmatine in test sample is calculated according to chromatogram,
Wherein, chromatographic condition is as follows：
Number of theoretical plate is calculated by tetrahydropalmatine peak should be not less than 3000, and chromatographic column uses octadecylsilane bonded silica
Glue is filler, and mobile phase is the acetonitrile-triethylamine aqueous solution, and the volume ratio of triethylamine is in its reclaimed water phase
0.01~0.03%, using gradient elution, Detection wavelength is 265-295nm, 25-45 DEG C of column temperature.
2. method according to claim 1, it is characterised in that Detection wavelength is 280nm.
3. method according to claim 1, it is characterised in that 35 DEG C of column temperature.
4. method according to claim 1, it is characterised in that gradient elution program is as follows：
5. method according to claim 1, it is characterised in that the wherein preparation of reference substance solution described in step 1,
Method is as follows：Tetrahydropalmatine reference substance plus methyl alcohol are taken, the solution of every 1ml μ containing 5-20 g is made.
6. method according to claim 5, it is characterised in that the wherein preparation of reference substance solution described in step 1,
Method is as follows：Tetrahydropalmatine reference substance plus methyl alcohol are taken, solution of every 1ml containing 10 μ g is made.
7. method according to claim 1, it is characterised in that the preparation of need testing solution wherein described in step 2,
Method is as follows：Test sample is finely ground, takes 0.1-1g plus Diluted Alcohol 5-20ml, ultrasonically treated more than 15min, puts
It is cold, plus filtered after Diluted Alcohol dilution, subsequent filtrate is taken, obtain final product.
8. method according to claim 7, it is characterised in that the preparation of need testing solution wherein described in step 2,
Method is as follows：Test sample is finely ground, takes 0.3g, accurately weighed, in putting 10ml measuring bottles, plus Diluted Alcohol about 8ml,
Ultrasonically treated 15 minutes, let cool, plus Diluted Alcohol is diluted to scale, shakes up, filtration, takes subsequent filtrate, obtains final product.
9. method according to claim 1, it is characterised in that the method for wherein step 3 is as follows：Control is taken respectively
Product solution 5-20 μ l, need testing solution 5-20 μ l, inject liquid chromatograph, obtain chromatogram, use external standard
One point method calculates the content of tetrahydropalmatine.
10. method according to claim 1, it is characterised in that step is as follows：
The wherein preparation of reference substance solution described in step 1, method is as follows：Weigh tetrahydropalmatine reference substance appropriate,
Plus methyl alcohol is made solution of every 1ml containing 10 μ g, obtains final product；
The preparation of need testing solution wherein described in step 2, method is as follows：Test sample is taken, it is finely ground, 0.3g is taken,
It is accurately weighed, in putting 10ml measuring bottles, plus Diluted Alcohol about 8ml, ultrasonically treated 15 minutes, let cool, plus dilute second
Alcohol is diluted to scale, shakes up, filtration, takes subsequent filtrate, obtains final product；
The method of wherein step 3 is as follows：Reference substance solution and each 10 μ l of need testing solution are drawn respectively, inject liquid
Chromatography, determines, and obtains final product；
Wherein, chromatographic condition is as follows：
Instrument uses Waters e2695 high performance liquid chromatographs；Waters Empower Pro work stations, Waters
2998 type UV-detectors, chromatographic condition is：It is filler with octadecylsilane chemically bonded silica；Acetonitrile -0.02%
Triethylamine water is mobile phase, gradient elution；Detection wavelength is 280nm, 35 DEG C of column temperature, and number of theoretical plate is by prolonging
Hu Suo Yisu peaks are calculated and should be not less than 3000,
Gradient elution program
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| CN108872462A (en) * | 2018-05-31 | 2018-11-23 | 广东万年青制药有限公司 | A kind of detection method of treasure China fir reason stomach piece |
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| CN108872462A (en) * | 2018-05-31 | 2018-11-23 | 广东万年青制药有限公司 | A kind of detection method of treasure China fir reason stomach piece |
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