CN104914194A - Method for detecting menthol content of peppermint oil drop pill by gas chromatograph - Google Patents
Method for detecting menthol content of peppermint oil drop pill by gas chromatograph Download PDFInfo
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Abstract
The invention belongs to the technical field of drug mass measurement, and particularly relates to a method for detecting the menthol content of a peppermint oil drop pill by a gas chromatograph. The method includes the steps: preparing menthol reference substance solution, preparing test article solution and sucking the menthol reference substance solution; injecting the menthol reference substance solution into the gas chromatograph and measuring peak area; drawing a standard curve to obtain a standard curve regression equation; sucking the test article solution; injecting the test article solution into the gas chromatograph for measurement; recording a chromatogram map; calculating the menthol content by an external standard method or the standard curve regression equation in the step (3). A capillary column with polyethylene glycol 20000 serving as a fixed phase is arranged in the gas chromatograph, the split ratio is 10-20:1, the initial temperature of the column is 50-115 DEG C and kept for 4-5 minutes, the temperature rises to reach 200 DEG C by 1.5-4 DEG C per minute and is kept for 2-3 minutes, the temperature of an injection port is 230 DEG C, the temperature of a detector is 230 DEG C, and carrier gas flow is 1-2ml/min.
Description
Technical field
The invention belongs to drug quality assay method technical field, be specially a kind of method that gas chromatograph detects Determination of menthol in Dementholized mint oil dripping pill.
Background technology
In Dementholized mint oil dripping pill, principal ingredient is peppermint oil dementholized, and peppermint oil dementholized Main Ingredients and Appearance is menthol (menthol), and therefore assay is selected with menthol is testing index.By the mensuration to Determination of menthol in Dementholized mint oil dripping pill, its quality be can effectively control, validity and the security of clinical application ensured.Menthol, be a kind of white strip or column crystallization, be monoterpenes composition, boiling point is lower, volatile, is insoluble in water, is soluble in ethanol, ester etc., makes water-soluble preparation and there is certain difficulty.
Detect Determination of menthol in Dementholized mint oil dripping pill, conventional detection method uses internal standard method to measure its content, and operating process is more complicated, and need to use internal standard compound, and cost is high.
Someone uses gas chromatograph to carry out the examination and analysb of raw material composition now, and gas chromatograph is a kind of separation, analysis tool of many mixture, and it take gas as mobile phase, adopts the Column chromatography techniques of douche.When the amalyzing substances of many components enters into chromatographic column, because each component gas phase is in the chromatography column different with the partition factor between immobile liquid liquid phase, therefore each component is also just different in the travelling speed of chromatographic column, after certain column length, order is left chromatographic column and is entered detecting device, be converted to electric signal after testing afterwards and deliver to data processing stations, thus complete the qualitative and quantitative analysis to measured matter.
But adopt vapor-phase chromatography to set up content assaying method, standard operating procedure is not only the simple operation steps really such as start, shutdown of instrument.Different material kind has different crucial location parameters, and different crucial location parameters can obtain different testing results.
At present also not about the relevant report detecting Determination of menthol in Dementholized mint oil dripping pill with gas chromatograph.Can therefore, detect Determination of menthol in Dementholized mint oil dripping pill with gas chromatograph? in mensuration process, how to select the location parameter being applicable to Determination of menthol? and how to make to choose the degree of separation of target peak, condition that symmetry, theoretical cam curve all can reach pharmacopoeial requirements? etc..These problems are then unknown at present, need to go to explore.
Summary of the invention
In order to solve above technical matters, the invention provides a kind of method that gas chromatograph detects Determination of menthol in Dementholized mint oil dripping pill, the method is simple to operate, and repeatability is high, and good stability, testing cost is low.
A kind of gas chromatograph solving above technical matters detects the method for Determination of menthol in Dementholized mint oil dripping pill, it is characterized in that: comprise the following steps:
(1) menthol reference substance solution is prepared: prepare menthol reference substance solution: get menthol reference substance, weighed, add ethanol and make; Be specially and get menthol reference substance, accurately weighed, add absolute ethyl alcohol and make the solution of every 1ml containing 0.2-0.52mg menthol, to obtain final product.
(2) prepare need testing solution: get test sample, weighedly put in measuring bottle, add water and ethanol, filter and get final product;
Be specially and get test sample, accurately weighed, put in measuring bottle, add water, ultrasonic process makes to leach, and adds absolute ethyl alcohol, and ultrasonic process 4-5 minute, lets cool, and adds absolute ethyl alcohol to required scale, shakes up, filter, get subsequent filtrate, to obtain final product;
(3) draw A, B, C, D and E menthol reference substance solution of different volumes, inject gas chromatograph, measure peak area, take sample size as horizontal ordinate, take peak area value as ordinate, carry out linear regression calculating, drawing standard curve, obtain typical curve regression equation, Y=nX+4e-13, X are sample size, and Y is peak area, n is slope, and 4E-13 is 4*10
-13science counting;
(4) draw need testing solution, inject gas chromatograph, measure, record chromatogram, calculates the content of menthol by external standard method; Or the content of menthol is gone out according to the typical curve regression equation calculation in step (3);
Wherein, in prioritization scheme of the present invention, be the capillary column of Stationary liquid with PEG 20000 in described gas chromatograph; Split sampling, split ratio 10-20:1; Column temperature is temperature programme, initial temperature 50-115 DEG C, keeps 4-5 minute, with the ramp to 200 DEG C of 1.5-4 per minute DEG C, keeps 2-3 minute; Injector temperature 230 DEG C; Detector temperature 230 DEG C; Carrier gas flux 1-2ml/min.
Also have in prioritization scheme, ultrasonic power 200W, frequency 40kHz in described ultrasonic process.
Described capillary column column length is 30m, and internal diameter is 0.53mm, and film thickness is 1 μm.
Described split ratio is 10:1, and split ratio is that the chromatographic peak peak shape of 10:1 is the most symmetrical, and degree of separation is best, and the number of plates is the highest.
The chromatographic peak peak shape of described carrier gas flux 2ml/min is the most symmetrical, and degree of separation is best.
Described column temperature is temperature programme: initial temperature 80-115 DEG C, keeps 4-5 minute, with the ramp to 200 DEG C of 3-4 per minute DEG C, keeps 3 minutes; Injector temperature 230 DEG C.
In further prioritization scheme, described column temperature is temperature programme: initial temperature 115 DEG C, keeps 5 minutes, with the ramp to 200 DEG C of 4 DEG C per minute, keeps 3 minutes; Injector temperature 230 DEG C.
Press menthol peak in described detection method to calculate, theoretical plate tower number is not less than 50000.
In testing process of the present invention, each absorption need testing solution amount is 1 μ 1.
In order to the flow process that simplifies the operation, adopt external standard method to carry out assay to Dementholized mint oil dripping pill in the present invention, by the mensuration to Determination of menthol in Dementholized mint oil dripping pill, effective its quality of control, ensures validity and the security of clinical application.
Menthol is monoterpenes composition, and boiling point is lower, adopts vapor-phase chromatography to set up content assaying method.Wherein column temperature, flow rate of carrier gas, split ratio are key parameter.Column temperature, the different appearance time of flow rate of carrier gas, the symmetry of target peak, degree of separation, theoretical cam curve are different; Split ratio is different, and the sample size entering instrument is different, and split ratio is large, and the sample size entering instrument is large, and split ratio is little, and the sample size entering instrument is little.
Gas chromatograph requires that each composition of sample carrying out instrument all has volatility, and when selective solvent, prioritizing selection has volatility, the solvent that toxicity is little, and through the contrast of multi-solvents, final absolute ethyl alcohol of selecting is as Extraction solvent.
The number of theoretical plate of the detection method in the present invention is 157833, degree of separation position 1.52, repeatability be 1% and tailing factor be 1.03, all reach the regulation in " Chinese Pharmacopoeia " version in 2010 annex VI D high performance liquid chromatography.
Accompanying drawing explanation
Fig. 1 is the courage drop pills canonical plotting of embodiment 5 in the present invention
Fig. 2-1,2-2,2-3 is that in the present invention, specificity investigates chromatogram
In figure, R is related coefficient, and X is sample size, and Y is peak area, and n is slope, and 4E-13 is 4*10
-13science counting
Embodiment
Below by way of example, the present invention is further illustrated, wherein:
Experimental apparatus used is Agilent 78090B gas chromatograph; Chromatographic column: HP-INNOWAX capillary column (30m*0.53mm*1 μm); Ten thousand/balance (Sai Duolisi BS110S), KQ-250B type ultrasonic cleaning machine (Kunshan ultrasonic electronic company limited).
Agents useful for same and reagent: water is ultrapure water, absolute ethyl alcohol is pure for analyzing.
Menthol is Nat'l Pharmaceutical & Biological Products Control Institute 110728-200506;
Courage drop pills: Sichuan New-green Pharmaceutical Technology Development Co., Ltd., lot number is 1312001,312002,1312003,140501,140502,140503,150401,150402,150403.
Embodiment 1
Gas chromatograph detects a method for Determination of menthol in Dementholized mint oil dripping pill, comprises the following steps:
(1) reference substance solution is prepared: get menthol reference substance, accurately weighed, add absolute ethyl alcohol and make the solution of every 1ml containing 0.2mg, to obtain final product.
(2) prepare need testing solution: get this product 5 ball, accurately weighed, put in 50ml measuring bottle, add water 4ml, and ultrasonic process makes to leach, add absolute ethyl alcohol 30ml, ultrasonic process (power 200W, frequency 40kHz) 5 minutes, lets cool, adds absolute ethyl alcohol to scale, shake up, filter, get subsequent filtrate, to obtain final product;
The matrix of courage drop pills is Macrogol 6000, easily molten in water or ethanol, peppermint oil dementholized can mix arbitrarily with ethanol, chloroform or ether, in the middle of mensuration process, a large amount of water inlet sample is larger to capillary column damage simultaneously, therefore determines the preparation method of courage drop pills collection of illustrative plates need testing solution in the present invention.
(3) precision draws 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 respectively, inject gas chromatograph, measuring peak area, take sample size as horizontal ordinate, be that ordinate carries out linear regression calculating with peak area value, drawing standard curve, obtains typical curve regression equation, Y=nX+4e-13, X(μ g) be sample size, Y is peak area, and n is slope, and 4E-13 is 4*10
-13science counting;
Be the capillary column (column length is 30m, and internal diameter is 0.53mm, and film thickness is 1 μm) of Stationary liquid with PEG 20000 in gas chromatograph; Column temperature is temperature programme: initial temperature 50 DEG C, keeps 5 minutes, with the ramp to 200 DEG C of 1.5 DEG C per minute, keeps 3 minutes; Injector temperature 230 DEG C; Detector temperature 230 DEG C; Split sampling, split ratio 10:1; Carrier gas flux 1.5ml/min; Number of theoretical plate calculates should be not less than 50 000 by menthol peak.
(4) each 1 μ 1 of accurate absorption need testing solution, inject gas chromatograph, measures, and record chromatogram, calculates the content of menthol by external standard method; Or the content of menthol is gone out according to the typical curve regression equation calculation in step (3).
Embodiment 2
Gas chromatograph detects a method for Determination of menthol in Dementholized mint oil dripping pill, other content as embodiment 1, wherein:
Preparation reference substance solution: get menthol reference substance, accurately weighed, add absolute ethyl alcohol and make the solution of every 1ml containing 0.52mg, to obtain final product.
Be the capillary column (column length is 30m, and internal diameter is 0.53mm, and film thickness is 1 μm) of Stationary liquid with PEG 20000 in gas chromatograph; Column temperature is temperature programme: initial temperature 60 DEG C, keeps 4 minutes, with the ramp to 200 DEG C of 3 DEG C per minute, keeps 3 minutes; Injector temperature 230 DEG C; Detector temperature 230 DEG C; Split sampling, split ratio 20:1; Carrier gas flux 2ml/min; Number of theoretical plate calculates should be not less than 50000 by menthol peak.
Embodiment 3
Gas chromatograph detects a method for Determination of menthol in Dementholized mint oil dripping pill, other content as embodiment 1, wherein:
Be the capillary column (column length is 30m, and internal diameter is 0.53mm, and film thickness is 1 μm) of Stationary liquid with PEG 20000 in gas chromatograph; Column temperature is temperature programme: initial temperature 80 DEG C, keeps 4 minutes, with the ramp to 200 DEG C of 3.5 DEG C per minute, keeps 2 minutes; Injector temperature 230 DEG C; Detector temperature 230 DEG C; Split sampling, split ratio 15:1; Carrier gas flux 1ml/min; Number of theoretical plate calculates should be not less than 50000 by menthol peak.
Embodiment 4
A kind of gas chromatograph detects the method for Determination of menthol in Dementholized mint oil dripping pill, other content is as embodiment 1, be wherein the capillary column (column length is 30m, and internal diameter is 0.53mm, and film thickness is 1 μm) of Stationary liquid with PEG 20000 in gas chromatograph; Column temperature is temperature programme: initial temperature 100 DEG C, keeps 5 minutes, with the ramp to 200 DEG C of 2.5 DEG C per minute, keeps 3 minutes; Injector temperature 230 DEG C; Detector temperature 230 DEG C; Split sampling, split ratio 12:1; Carrier gas flux 2ml/min; Number of theoretical plate calculates should be not less than 50000 by menthol peak.
Embodiment 5
Gas chromatograph detects a method for Determination of menthol in Dementholized mint oil dripping pill, other content as embodiment 1,
Preparation reference substance solution: get menthol reference substance, accurately weighed, add absolute ethyl alcohol and make the solution of every 1ml containing 0.52mg, to obtain final product.
Be wherein the capillary column (column length is 30m, and internal diameter is 0.53mm, and film thickness is 1 μm) of Stationary liquid with PEG 20000 in gas chromatograph; Column temperature is temperature programme: initial temperature 115 DEG C, keeps 5 minutes, with the ramp to 200 DEG C of 4 DEG C per minute, keeps 3 minutes; Injector temperature 230 DEG C; Detector temperature 230 DEG C; Split sampling, split ratio 10:1; Carrier gas flux 2ml/min; Number of theoretical plate calculates should be not less than 50000 by menthol peak.
Typical curve regression equation is: in Y=1.827.3X+4E-13, figure, R is related coefficient, is used for the degree of metric linear correlativity, more more illustrates that linear dependence is better close to 1.
Result is as table 1 and Fig. 1:
Table 1 menthol typical curve result table
Result shows: menthol sample size is within the scope of 0.1 ~ 0.75 μ g, and sample size and peak area value are good linear relationship.
Test one: different column temperature and heating schedule are on the impact of assay
With embodiment 5 for experimental group, set up control group 1,2 and 3, specific as follows:
Control group 1: other content is as embodiment 5, and column temperature initial temperature 80 DEG C, keeps 5 minutes, with the ramp to 115 DEG C of 10 DEG C per minute, keeps 5 minutes, with the ramp to 200 DEG C of 4 DEG C per minute, keeps 3 minutes; Injector temperature 230 DEG C; Detector temperature 230 DEG C;
Control group 2: other content is as embodiment 5, and column temperature initial temperature 50 DEG C, keeps 5 minutes, with the ramp to 135 DEG C of 1.5 DEG C per minute, then with the ramp to 200 DEG C of 30 DEG C per minute; Injector temperature 230 DEG C; Detector temperature 230 DEG C.
Control group 3: other content is as embodiment 5, and column temperature initial temperature 60 DEG C, keeps 4 minutes, with the ramp to 130 DEG C of 1.5 DEG C per minute, then with the ramp to 200 DEG C of 20 DEG C per minute; Injector temperature 250 DEG C; Detector temperature 250 DEG C.
Result is as table 2:
Table 2 chromatography condition result
Result shows: the menthol peak degree of separation in experimental group, symmetrical factor, the number of plates all reach Chinese Pharmacopoeia requirement, and working time is relatively short, so the column temperature in the present invention is effective.
Test two: stability of solution is tested
Operation steps, as embodiment 5, gets the need testing solution prepared, and respectively at 0,2,6,12,18,24 hour sample introduction, record menthol peak area, calculated RSD, the results are shown in Table 3.
Table 3 stability test result
Above result shows: under this experiment condition, and sample test liquid is good at 24 hours internal stabilities.
Test three: the specificity of the detection method in the present invention is investigated
Prepare need testing solution and the negative solution of scarce peppermint oil dementholized (not containing peppermint oil dementholized) by the method in embodiment 5, the mensuration of the negative solution chromatogram of result to peak to be measured is noiseless, shows that the method specificity is good.See Fig. 2-1,2-2,2-3.
Test four: sample introduction Precision Experiment
Operation steps is as embodiment 5, and accurate absorption menthol reference substance solution (menthol 0.52mg/ml) 1 μ l, continuous sample introduction 6 times, record peak area, calculates RSD, the results are shown in Table 4.
Table 4 sample introduction Precision test result table
Result shows that the detection method sample introduction precision in the present invention is good.
Test five: Intermediate precision is tested
Operation steps, as embodiment 5, gets with a collection of test sample that (lot number: 1312001), respectively by A, B two people, at different time, each process three increment product, measure the content of this product menthol by content assaying method with same equipment, calculate RSD.The results are shown in Table 5.
Menthol Intermediate precision result table
Result shows: the detection method Intermediate precision in the present invention is good.
Test six: replica test
Operation steps is as embodiment 5, and (lot number: 1312001) powder 5 ball, puts in tool plug conical flask by totally 6 parts, according to the method preparation drafted and mensuration, the results are shown in Table 6 to get this product.
Table 6 menthol replica test result
Result shows: the detection repeatability in the present invention is good.
Test seven: average recovery is tested
Operation steps is as embodiment 5, get the sample (lot number: 1312001 of known content, the content 1.95mg/ ball of menthol,) 3 balls, totally 6 parts, accurately weighed, precision adds menthol reference substance solution (0.52mg/ml) 10ml respectively, prepare by the method drafted and measure, calculating the recovery, the results are shown in Table 7.Computing formula as
Under:
Table 7 menthol recovery test result
Result shows: the detection method accuracy in the present invention is good.
Detection method in the present invention, under existing instrument condition, simplify the operation flow process, measures menthol by external standard method, and result appearance method detects indifference in check result final with by the internal standard method of classic method.Detecting Determination of menthol with gas chromatograph in the present invention, is full-automatic sample introduction, and sampling volume reappearance is fine, also has good analytical precision without internal standard method, and simple to operate, and cost is low, and repeatability, stability is high.
Claims (9)
1. detect a method for Determination of menthol in Dementholized mint oil dripping pill with gas chromatograph, it is characterized in that: comprise the following steps:
(1) menthol reference substance solution is prepared: get menthol reference substance, weighed, add ethanol and make;
(2) prepare need testing solution: get test sample, weighedly put in measuring bottle, add water and ethanol, filter and get final product;
(3) draw A, B, C, D and E menthol reference substance solution of different volumes, inject gas chromatograph, measure peak area, take sample size as horizontal ordinate, take peak area value as ordinate, carry out linear regression calculating, drawing standard curve, obtain typical curve regression equation, Y=nX+4E-13, X are sample size, and Y is peak area, n is slope, and 4E-13 is 4*10
-13science counting;
(4) draw need testing solution, inject gas chromatograph, measure, record chromatogram, calculates the content of menthol by external standard method; Or the content of menthol is gone out according to the typical curve regression equation calculation in step (3).
2. a kind of gas chromatograph according to claim 1 detects the method for Determination of menthol in Dementholized mint oil dripping pill, it is characterized in that: the capillary column in described gas chromatograph with PEG 20000 being Stationary liquid; Split sampling, split ratio 10-20:1; Column temperature is temperature programme, initial temperature 50-115 DEG C, keeps 4-5 minute, with the ramp to 200 DEG C of 1.5-4 per minute DEG C, keeps 2-3 minute; Injector temperature 230 DEG C; Detector temperature 230 DEG C; Carrier gas flux 1-2ml/min.
3. a kind of gas chromatograph according to claim 2 detects the method for Determination of menthol in Dementholized mint oil dripping pill, it is characterized in that: ultrasonic power 200W, frequency 40kHz in described ultrasonic process.
4. a kind of gas chromatograph according to claim 2 detects the method for Determination of menthol in Dementholized mint oil dripping pill, and it is characterized in that: described capillary column column length is 30m, internal diameter is 0.53mm, and film thickness is 1 μm.
5. a kind of gas chromatograph according to claim 2 detects the method for Determination of menthol in Dementholized mint oil dripping pill, it is characterized in that: described split ratio is 10:1.
6. a kind of gas chromatograph according to claim 2 detects the method for Determination of menthol in Dementholized mint oil dripping pill, it is characterized in that: described carrier gas flux 2ml/min.
7. a kind of gas chromatograph according to claim 2 detects the method for Determination of menthol in Dementholized mint oil dripping pill, it is characterized in that: described column temperature is temperature programme: initial temperature 80-115 DEG C, keep 4-5 minute, with the ramp to 200 DEG C of 3-4 per minute DEG C, keep 3 minutes; Injector temperature 230 DEG C.
8. a kind of gas chromatograph according to claim 7 detects the method for Determination of menthol in Dementholized mint oil dripping pill, it is characterized in that: described column temperature is temperature programme: initial temperature 115 DEG C, keep 5 minutes, with the ramp to 200 DEG C of 4 DEG C per minute, keep 3 minutes; Injector temperature 230 DEG C.
9. a kind of gas chromatograph according to claim 1 detects the method for Determination of menthol in Dementholized mint oil dripping pill, it is characterized in that: calculate by menthol peak in described detection method, theoretical plate tower number is not less than 50000.
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