CN104914194B - A method of with Determination of menthol in gas chromatograph detection Dementholized mint oil dripping pill - Google Patents
A method of with Determination of menthol in gas chromatograph detection Dementholized mint oil dripping pill Download PDFInfo
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Abstract
The invention belongs to drug quality measuring method technical fields, specially a kind of method with Determination of menthol in gas chromatograph detection Dementholized mint oil dripping pill, including preparing menthol reference substance solution, preparing test solution, absorption menthol reference substance solution, inject gas chromatograph, measure peak area, standard curve is drawn, standard curve regression equation is obtained；Test solution is drawn again, injects gas chromatograph for determination, records chromatogram, and the content of menthol is calculated with external standard method；Or go out the content of menthol with the standard curve regression equation calculation in step (3)；Wherein using PEG 20000 as the capillary column of stationary phase in gas chromatograph；Split ratio 10-20:1；50-115 DEG C of column temperature initial temperature is kept for 4-5 minutes, is warming up to 200 DEG C with 1.5-4 DEG C per minute of rate, is kept for 2-3 minutes；230 DEG C of injector temperature；230 DEG C of detector temperature；Carrier gas flux 1-2ml/min.
Description
Technical field
It is specially a kind of to detect peppermint oil dementholized with gas chromatograph the invention belongs to drug quality measuring method technical field
The method of Determination of menthol in dripping pill.
Background technique
Main component is peppermint oil dementholized in Dementholized mint oil dripping pill, and peppermint oil dementholized main ingredient is menthol (menthol), because
This assay is selected using menthol as testing index.Pass through the measurement to Determination of menthol in Dementholized mint oil dripping pill, Neng Gouyou
Its quality of the control of effect guarantees the validity and safety of clinical application.Menthol, is a kind of white strip or column crystallization,
For monoterpene constituents, boiling point is lower, volatile, is insoluble in water, is soluble in ethyl alcohol, ester etc., and water-soluble preparation is made and exists centainly
Difficulty.
Determination of menthol in Dementholized mint oil dripping pill is detected, common detection method is to survey using internal standard method to its content
Fixed, operating process is more complex, and it also requires using internal standard compound, it is at high cost.
Present someone carries out the detection and analysis of raw material composition with gas chromatograph, and gas chromatograph is a kind of multiple groups
Part mixture separates, analyzes tool, it is using gas as mobile phase, using the Column chromatography techniques of douche.When multiple groups part
When analysis substance enters chromatographic column, not due to the distribution coefficient between the gas phase and fixer liquid phase of each component in the chromatography column
Together, therefore each component is also just different in the speed of service of chromatographic column, after certain column length, sequentially leaves chromatographic column and enters inspection
Device is surveyed, electric signal is converted to after detecting and is sent to data processing stations, so as to complete the qualitative, quantitative to measured matter point
Analysis.
But content assaying method is established using gas chromatography, standard operating procedure is not only the booting of instrument, shutdown
Deng simple operating procedure really.Different material type has different crucial location parameters, and different crucial location parameters can obtain
To different testing results.
There is presently no about the relevant report with Determination of menthol in gas chromatograph detection Dementholized mint oil dripping pill.Cause
This, if Determination of menthol in Dementholized mint oil dripping pill can be detected with gas chromatograph how to select to be suitble in continuous mode
The location parameter of Determination of menthol and reach separating degree, symmetry, the theoretical cam curve of choosing target peak can all
The condition of pharmacopoeial requirements etc..These problems be then at present it is unknown, need to explore.
Summary of the invention
In order to solve the above technical problems, the present invention provide it is a kind of with gas chromatograph detection Dementholized mint oil dripping pill in peppermint
The method of brain content, the method is easy to operate, and repeatability is high, and stability is good, and testing cost is low.
A kind of method with Determination of menthol in gas chromatograph detection Dementholized mint oil dripping pill of the above technical problem is solved,
It is characterized by comprising following steps:
(1) it prepares menthol reference substance solution: preparing menthol reference substance solution: taking menthol reference substance, it is weighed, add second
Alcohol is made；Menthol reference substance is specially taken, it is accurately weighed, add dehydrated alcohol that every 1ml menthol containing 0.2-0.52mg is made
Solution to get.
(2) it prepares test solution: taking test sample, it is weighed to set in measuring bottle, add water and ethyl alcohol, filter to obtain the final product；
Test sample is specially taken, it is accurately weighed, it sets in measuring bottle, adds water, ultrasonic treatment makes to leach, and dehydrated alcohol is added, and surpasses
Sonication 4-5 minutes, let cool, dehydrated alcohol added to shake up to required scale, filter, take subsequent filtrate to get；
(3) A, B, C, D and E the menthol reference substance solution for drawing different volumes, inject gas chromatograph, measure peak face
Product using peak area value as ordinate, carries out linear regression calculating, draws standard curve, obtain standard using sample volume as abscissa
Regression Equations, Y=nX+4e-13, X are sample volume, and Y is peak area, and n is slope, 4E-13 4*10-13Science count；
(4) test solution is drawn, gas chromatograph is injected, measurement records chromatogram, calculates menthol with external standard method
Content；Or go out the content of menthol according to the standard curve regression equation calculation in step (3)；
Wherein, in prioritization scheme of the invention, using PEG 20000 as the capillary of stationary phase in the gas chromatograph
Tubing string；Split sampling, split ratio 10-20:1；Column temperature is temperature programming, 50-115 DEG C of initial temperature, is kept for 4-5 minutes, with every
The rate of 1.5-4 DEG C of minute is warming up to 200 DEG C, is kept for 2-3 minutes；230 DEG C of injector temperature；230 DEG C of detector temperature；Carrier gas
Flow 1-2ml/min.
There are also in prioritization scheme, ultrasonic power 200W, frequency 40kHz in the ultrasonic treatment.
The capillary column column length is 30m, and internal diameter 0.53mm, film thickness is 1 μm.
The split ratio is 10:1, and split ratio is that the chromatographic peak peak shape of 10:1 is the most symmetrical, and separating degree is best, and the number of plates is most
It is high.
The chromatographic peak peak shape of the carrier gas flux 2ml/min is the most symmetrical, and separating degree is best.
The column temperature is temperature programming: 80-115 DEG C of initial temperature, being kept for 4-5 minutes, with 3-4 DEG C per minute of rate liter
Temperature is kept for 3 minutes to 200 DEG C；230 DEG C of injector temperature.
It advanced optimizes in scheme, the column temperature is temperature programming: 115 DEG C of initial temperature, being kept for 5 minutes, with per minute 4
DEG C rate be warming up to 200 DEG C, kept for 3 minutes；230 DEG C of injector temperature.
It is calculated in the detection method by menthol peak, theoretical plate tower number is not less than 50000.
Drawing test solution amount in detection process of the invention every time is 1 μ 1.
For streamline operation, assay is carried out to Dementholized mint oil dripping pill using external standard method in the present invention, by right
The measurement of Determination of menthol in Dementholized mint oil dripping pill, effectively controls its quality, guarantees the validity and safety of clinical application.
Menthol is monoterpene constituents, and boiling point is lower, establishes content assaying method using gas chromatography.Wherein column temperature,
Flow rate of carrier gas, split ratio are key parameter.Column temperature, flow rate of carrier gas difference appearance time, the symmetry of target peak, separating degree, reason
By number of plates difference；Split ratio is different, and the sample size into instrument is different, and split ratio is big, and the sample size into instrument is big, shunts
Than small, the sample size into instrument is small.
Gas chromatograph requires each ingredient of sample for carrying out instrument to all have volatility, preferentially selects to have when selecting solvent
There is volatility, the solvent of small toxicity, by the comparison of multi-solvents, final choice dehydrated alcohol is as Extraction solvent.
The number of theoretical plate of detection method in the present invention is 157833, separating degree position 1.52, repeatability are 1% and hangover because
Son is 1.03, reaches the regulation in one annex of " Chinese Pharmacopoeia " version in 2010, VI D high performance liquid chromatography.
Detailed description of the invention
Fig. 1 is the gallbladder drop pills canonical plotting of embodiment 5 in the present invention
Fig. 2-1,2-2,2-3 are that specificity investigates chromatogram in the present invention
R is related coefficient in figure, and X is sample volume, and Y is peak area, and n is slope, 4E-13 4*10-13Science count
Specific embodiment
Below by way of example, the present invention is further illustrated, in which:
Laboratory apparatus used is Agilent 78090B gas chromatograph；Chromatographic column: HP-INNOWAX capillary column (30m*
0.53mm*1 μm)；A ten thousandth balance (Sai Duolisi BS110S), (Kunshan ultrasonic electronic has KQ-250B type ultrasonic cleaning machine
Limit company).
Agents useful for same and reagent: water is ultrapure water, and dehydrated alcohol is that analysis is pure.
Menthol is Nat'l Pharmaceutical & Biological Products Control Institute 110728-200506；
Gallbladder drop pills: Sichuan New-green Pharmaceutical Technology Development Co., Ltd., lot number 1312001,312002,
1312003,140501,140502,140503,150401,150402,150403.
Embodiment 1
A method of with Determination of menthol in gas chromatograph detection Dementholized mint oil dripping pill, comprising the following steps:
(1) it prepares reference substance solution: taking menthol reference substance, it is accurately weighed, add dehydrated alcohol that every 1ml is made containing 0.2mg
Solution to get.
(2) it prepares test solution: taking 5 ball of this product, it is accurately weighed, it sets in 50ml measuring bottle, adds water 4ml, ultrasonic treatment makes
It leaches, dehydrated alcohol 30ml is added, ultrasonic treatment (power 200W, frequency 40kHz) 5 minutes is let cool, and adds dehydrated alcohol to quarter
Degree, shake up, filter, take subsequent filtrate to get；
The matrix of gallbladder drop pills is Macrogol 6000, readily soluble in water or ethyl alcohol, peppermint oil dementholized and ethyl alcohol, chloroform or second
Ether can be mixed arbitrarily, at the same sample of largely intaking in continuous mode capillary column is damaged it is bigger, it is thus determined that of the invention
The preparation method of middle gallbladder drop pills map test solution.
(3) accurate respectively to draw menthol reference substance solution (0.52mg/ml) 0.2 μ l, 0.5 μ l, 0.8 μ l, 1 μ l, 1.5 μ
L injects gas chromatograph, measures peak area, using sample volume as abscissa, carries out linear regression as ordinate using peak area value and counts
Calculate, draw standard curve, obtain standard curve regression equation, Y=nX+4e-13, X(μ g) it is sample volume, Y is peak area, and n is oblique
Rate, 4E-13 4*10-13Science count；
In gas chromatograph using PEG 20000 as stationary phase capillary column (column length 30m, internal diameter 0.53mm,
Film thickness is 1 μm)；Column temperature is temperature programming: 50 DEG C of initial temperature, being kept for 5 minutes, is warming up to 1.5 DEG C of rate per minute
It 200 DEG C, is kept for 3 minutes；230 DEG C of injector temperature；230 DEG C of detector temperature；Split sampling, split ratio 10:1；Carrier gas flux
1.5ml/min；Number of theoretical plate is calculated by menthol peak should be not less than 50 000.
(4) accurate to draw each 1 μ 1 of test solution, gas chromatograph is injected, measurement records chromatogram, with external standard method meter
Calculate the content of menthol；Or go out the content of menthol according to the standard curve regression equation calculation in step (3).
Embodiment 2
A method of with gas chromatograph detection Dementholized mint oil dripping pill in Determination of menthol, other contents such as embodiment 1,
Wherein:
Preparation reference substance solution: taking menthol reference substance, accurately weighed, adds dehydrated alcohol that every 1ml is made containing 0.52mg's
Solution to get.
In gas chromatograph using PEG 20000 as stationary phase capillary column (column length 30m, internal diameter 0.53mm,
Film thickness is 1 μm)；Column temperature is temperature programming: 60 DEG C of initial temperature, being kept for 4 minutes, is warming up to 200 with 3 DEG C of rate per minute
DEG C, it is kept for 3 minutes；230 DEG C of injector temperature；230 DEG C of detector temperature；Split sampling, split ratio 20:1；Carrier gas flux 2ml/
min；Number of theoretical plate is calculated by menthol peak should be not less than 50000.
Embodiment 3
A method of with gas chromatograph detection Dementholized mint oil dripping pill in Determination of menthol, other contents such as embodiment 1,
Wherein:
In gas chromatograph using PEG 20000 as stationary phase capillary column (column length 30m, internal diameter 0.53mm,
Film thickness is 1 μm)；Column temperature is temperature programming: 80 DEG C of initial temperature, being kept for 4 minutes, is warming up to 3.5 DEG C of rate per minute
It 200 DEG C, is kept for 2 minutes；230 DEG C of injector temperature；230 DEG C of detector temperature；Split sampling, split ratio 15:1；Carrier gas flux
1ml/min；Number of theoretical plate is calculated by menthol peak should be not less than 50000.
Embodiment 4
A method of with gas chromatograph detection Dementholized mint oil dripping pill in Determination of menthol, other contents such as embodiment 1,
Wherein using PEG 20000 as capillary column (column length 30m, internal diameter 0.53mm, the film thickness of stationary phase in gas chromatograph
Degree is 1 μm)；Column temperature is temperature programming: 100 DEG C of initial temperature, being kept for 5 minutes, is warming up to 200 with 2.5 DEG C of rate per minute
DEG C, it is kept for 3 minutes；230 DEG C of injector temperature；230 DEG C of detector temperature；Split sampling, split ratio 12:1；Carrier gas flux 2ml/
min；Number of theoretical plate is calculated by menthol peak should be not less than 50000.
Embodiment 5
A method of with gas chromatograph detection Dementholized mint oil dripping pill in Determination of menthol, other contents such as embodiment 1,
Preparation reference substance solution: taking menthol reference substance, accurately weighed, adds dehydrated alcohol that every 1ml is made containing 0.52mg's
Solution to get.
Wherein using PEG 20000 as the capillary column of stationary phase, (column length 30m, internal diameter are in gas chromatograph
0.53mm, film thickness are 1 μm)；Column temperature is temperature programming: 115 DEG C of initial temperature, being kept for 5 minutes, with 4 DEG C of rate per minute
200 DEG C are warming up to, is kept for 3 minutes；230 DEG C of injector temperature；230 DEG C of detector temperature；Split sampling, split ratio 10:1；It carries
Throughput 2ml/min；Number of theoretical plate is calculated by menthol peak should be not less than 50000.
Standard curve regression equation are as follows: Y=1.827.3X+4E-13, R is related coefficient in figure, and it is related to be used to metric linear
Property degree, closer to 1 more illustrating that linear dependence is better.
As a result such as table 1 and Fig. 1:
1 menthol standard curve result table of table
The result shows that: menthol sample volume is in 0.1 ~ 0.75 μ g range, and sample volume and peak area value are in good linear
Relationship.
Test one: the influence of different column temperatures and temperature program to assay
It is experimental group with embodiment 5, sets up control group 1,2 and 3, specific as follows:
Control group 1: other contents such as embodiment 5, is kept for 5 minutes, with 10 DEG C of speed per minute by 80 DEG C of column temperature initial temperature
Rate is warming up to 115 DEG C, is kept for 5 minutes, is warming up to 200 DEG C with 4 DEG C of rate per minute, is kept for 3 minutes；Injector temperature 230
℃；230 DEG C of detector temperature；
Control group 2: other contents such as embodiment 5, is kept for 5 minutes, with 1.5 DEG C per minute by 50 DEG C of column temperature initial temperature
Rate is warming up to 135 DEG C, then is warming up to 200 DEG C with 30 DEG C of rate per minute；230 DEG C of injector temperature；Detector temperature 230
℃。
Control group 3: other contents such as embodiment 5, is kept for 4 minutes, with 1.5 DEG C per minute by 60 DEG C of column temperature initial temperature
Rate is warming up to 130 DEG C, then is warming up to 200 DEG C with 20 DEG C of rate per minute；250 DEG C of injector temperature；Detector temperature 250
℃。
As a result such as table 2:
2 chromatography condition result of table
As the result is shown: menthol peak separating degree, symmetrical factor, the number of plates in experimental group reach Chinese Pharmacopoeia requirement,
And runing time is relatively short, so the column temperature effect in the present invention is good.
Test two: stability of solution experiment
Operating procedure such as embodiment 5, takes the test solution prepared, respectively at 0,2,6,12,18,24 hour into
Sample records menthol peak area, calculates RSD, the results are shown in Table 3.
3 stability test result of table
The above result shows that: under this experiment condition, sample test liquid is good in 24 hours internal stabilities.
Test three: the specificity of the detection method in the present invention is investigated
Test solution and scarce peppermint oil dementholized feminine gender solution (without peppermint oil dementholized), knot are prepared by the method in embodiment 5
Fruit feminine gender solution chromatogram is noiseless to the measurement at peak to be measured, shows that this method specificity is good.See Fig. 2-1,2-2,2-3.
Test four: sample introduction Precision Experiment
Operating procedure such as embodiment 5, precision draw menthol reference substance solution (menthol 0.52mg/ml) 1 μ l, continuously into
Sample 6 times, peak area is recorded, RSD is calculated, the results are shown in Table 4.
4 sample introduction Precision test result table of table
The result shows that the detection method sample introduction precision in the present invention is good.
Test five: Intermediate precision experiment
Operating procedure such as embodiment 5 takes with a collection of test sample (lot number: 1312001), respectively by two people of A, B, when different
Between, three parts of samples are respectively handled, measure the content of this product menthol by content assaying method with same equipment, calculate RSD.As a result
It is shown in Table 5.
Menthol Intermediate precision result table
The result shows that: the detection method Intermediate precision in the present invention is good.
Test six: repetitive test
Operating procedure such as embodiment 5, taking this product, (lot number: 1312001) 5 ball of powder, is set in stuffed conical flask, is pressed by totally 6 parts
According to the method preparation and measurement drafted, it the results are shown in Table 6.
6 menthol repetitive test result of table
The result shows that: the detection repeatability in the present invention is good.
Test seven: sample recovery rate experiment
Operating procedure such as embodiment 5 takes the sample (lot number: 1312001, the content 1.95mg/ of menthol of known content
Ball) 3 balls, it is totally 6 parts, accurately weighed, it is accurate respectively that menthol reference substance solution (0.52mg/ml) 10ml is added, by the side drafted
Method is prepared and is measured, and is calculated the rate of recovery, be the results are shown in Table 7.Calculation formula is as follows:
7 menthol recovery test result of table
The result shows that: the detection method accuracy in the present invention is good.
Detection method in the present invention, under existing instrument condition, streamline operation carries out menthol with external standard method
Measurement, as a result appearance method is finally detecting the indifference in inspection result with the internal standard method of conventional method.Gas is used in the present invention
Chromatography detects Determination of menthol, is full-automatic sample introduction, and sampling volume reproducibility is fine, also has without internal standard method well
Analytical precision, and easy to operate, at low cost, repeatability, stability are high.
Claims (2)
1. a kind of method with Determination of menthol in gas chromatograph detection Dementholized mint oil dripping pill, it is characterised in that: including following
Step:
(1) it prepares menthol reference substance solution: taking menthol reference substance, it is weighed, add ethyl alcohol that every 1ml menthol containing 0.52mg is made
Solution；
(2) it prepares test solution: taking test sample, it is weighed to set in measuring bottle, add water, ultrasonic treatment to make to leach, add ethyl alcohol, at ultrasound
Reason 4-5 minutes, lets cool, adds dehydrated alcohol to required scale, shake up, filter to obtain the final product；
(3) A, B, C, D and E the menthol reference substance solution for drawing different volumes, inject gas chromatograph, measure peak area, with
Sample volume is abscissa, using peak area value as ordinate, carries out linear regression calculating, draws standard curve, obtain standard curve
Regression equation, Y=1827.3X+4E-13, X are sample volume, and Y is peak area, and the science that 4E-13 is 4*10-13 counts；
(4) test solution is drawn, gas chromatograph is injected, measurement records chromatogram, calculates containing for menthol with external standard method
Amount；Or go out the content of menthol according to the standard curve regression equation calculation in step (3)；
Using PEG 20000 as the capillary column of stationary phase in the gas chromatograph, column length 30m, internal diameter 0.53mm,
Film thickness is 1 μm；Split sampling, split ratio 10:1；Column temperature is temperature programming, 115 DEG C of initial temperature, is kept for 5 minutes, with every point
The rate that 4 DEG C of clock is warming up to 200 DEG C, is kept for 3 minutes；230 DEG C of injector temperature；230 DEG C of detector temperature；Carrier gas flux 2ml/
min；It is calculated by menthol peak, theoretical plate tower number is not less than 50000.
2. a kind of method with Determination of menthol in gas chromatograph detection Dementholized mint oil dripping pill according to claim 1,
It is characterized by: the carrier gas flux 2ml/min.
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| CN112924593B (en) * | 2021-02-04 | 2023-04-07 | 北京同仁堂制药有限公司 | Detection method for lasting brain strengthening effect |
| CN114441695A (en) * | 2022-01-26 | 2022-05-06 | 武汉九州钰民医药科技有限公司 | Method for detecting N, N-dimethylformamide in ceftazidime residual solvent and application |
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