CN116818946A - Method for measuring sorbic acid in simethicone emulsion by HPLC (high Performance liquid chromatography) - Google Patents
Method for measuring sorbic acid in simethicone emulsion by HPLC (high Performance liquid chromatography) Download PDFInfo
- Publication number
- CN116818946A CN116818946A CN202310800219.9A CN202310800219A CN116818946A CN 116818946 A CN116818946 A CN 116818946A CN 202310800219 A CN202310800219 A CN 202310800219A CN 116818946 A CN116818946 A CN 116818946A
- Authority
- CN
- China
- Prior art keywords
- sorbic acid
- simethicone emulsion
- solution
- hplc
- mobile phase
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- BEFDCLMNVWHSGT-UHFFFAOYSA-N ethenylcyclopentane Chemical compound C=CC1CCCC1 BEFDCLMNVWHSGT-UHFFFAOYSA-N 0.000 title claims abstract description 73
- 239000004334 sorbic acid Substances 0.000 title claims abstract description 73
- 229940075582 sorbic acid Drugs 0.000 title claims abstract description 73
- 235000010199 sorbic acid Nutrition 0.000 title claims abstract description 73
- 238000000034 method Methods 0.000 title claims abstract description 48
- AMTWCFIAVKBGOD-UHFFFAOYSA-N dioxosilane;methoxy-dimethyl-trimethylsilyloxysilane Chemical compound O=[Si]=O.CO[Si](C)(C)O[Si](C)(C)C AMTWCFIAVKBGOD-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000000839 emulsion Substances 0.000 title claims abstract description 42
- 229940083037 simethicone Drugs 0.000 title claims abstract description 42
- 238000004128 high performance liquid chromatography Methods 0.000 title claims abstract description 31
- 238000012360 testing method Methods 0.000 claims abstract description 37
- 238000005303 weighing Methods 0.000 claims abstract description 27
- 238000007865 diluting Methods 0.000 claims abstract description 22
- 239000012488 sample solution Substances 0.000 claims abstract description 21
- 238000001914 filtration Methods 0.000 claims abstract description 14
- 239000000523 sample Substances 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 239000012088 reference solution Substances 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims description 46
- 239000002904 solvent Substances 0.000 claims description 28
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 27
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 20
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 14
- 229940040526 anhydrous sodium acetate Drugs 0.000 claims description 14
- 239000007974 sodium acetate buffer Substances 0.000 claims description 13
- 238000004090 dissolution Methods 0.000 claims description 12
- 229960000583 acetic acid Drugs 0.000 claims description 10
- 239000012362 glacial acetic acid Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 239000000706 filtrate Substances 0.000 claims description 9
- 238000010828 elution Methods 0.000 claims description 8
- 238000010790 dilution Methods 0.000 claims description 7
- 239000012895 dilution Substances 0.000 claims description 7
- 239000000945 filler Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 238000003113 dilution method Methods 0.000 claims description 2
- 239000012085 test solution Substances 0.000 abstract description 14
- 238000005259 measurement Methods 0.000 abstract description 5
- 229940079593 drug Drugs 0.000 abstract description 4
- 239000003814 drug Substances 0.000 abstract description 4
- 235000014443 Pyrus communis Nutrition 0.000 abstract description 3
- 239000002253 acid Substances 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000035945 sensitivity Effects 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 3
- 238000001514 detection method Methods 0.000 abstract description 2
- 239000012071 phase Substances 0.000 description 17
- 239000013558 reference substance Substances 0.000 description 14
- 239000000047 product Substances 0.000 description 8
- 230000014759 maintenance of location Effects 0.000 description 5
- 239000012490 blank solution Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000011550 stock solution Substances 0.000 description 4
- 230000001276 controlling effect Effects 0.000 description 2
- 239000003085 diluting agent Substances 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000013112 stability test Methods 0.000 description 2
- 206010000060 Abdominal distension Diseases 0.000 description 1
- 230000003187 abdominal effect Effects 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000002872 contrast media Substances 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 210000001035 gastrointestinal tract Anatomy 0.000 description 1
- 238000002575 gastroscopy Methods 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- -1 polydimethylsiloxane Polymers 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the technical field of sorbic acid content measurement, in particular to a method for measuring sorbic acid in simethicone emulsion by an HPLC method; preparing a test sample, namely taking a proper amount of simethicone emulsion, precisely weighing, diluting, and filtering to obtain a test sample solution; preparing reference, namely taking a proper amount of sorbic acid reference, precisely weighing, and diluting to obtain a reference solution; detecting the content of the pear acid in the test solution by adopting an HPLC method; by the method, the sorbic acid in the simethicone emulsion can be accurately detected, the separation degree between the sorbic acid and adjacent peaks, the number of theoretical plates and the trailing factor symmetry factor are good, the response is high, the method is suitable for measuring the sorbic acid content in a multi-component preparation, the detection method is strong in specificity, high in sensitivity, stable and reliable, the method can be used for measuring the sorbic acid content in the simethicone emulsion and controlling the quality, and a beneficial reference is provided for the production process and medication safety.
Description
Technical Field
The invention relates to the technical field of sorbic acid content measurement, in particular to a method for measuring sorbic acid in simethicone emulsion by an HPLC method.
Background
Simethicone is a mixture of polydimethylsiloxane and silica; simethicone may also be used post-operatively to treat discomfort associated with excessive gas accumulation in the gastrointestinal tract (e.g., abdominal distension, etc.). In addition, the composition can be used as an auxiliary drug for abdominal imaging examination (such as X-ray, ultrasound and gastroscopy) and an additive of contrast agent suspension for dual contrast display.
Sorbic acid is used as a preservative in the preparation of simethicone emulsion, and the content of sorbic acid in each 1ml is 1.2mg according to the prescription amount. The existing sorbic acid content determination method is a titration method and is not suitable for multicomponent preparations, so that a liquid phase detection method with stronger specificity needs to be developed.
Disclosure of Invention
The invention aims to provide a method for measuring sorbic acid in simethicone emulsion by an HPLC method, and aims to solve the technical problem that the existing sorbic acid content measuring method in the prior art is not suitable for multicomponent preparations.
In order to achieve the above purpose, the method for measuring sorbic acid in simethicone emulsion by adopting an HPLC method comprises the following steps:
preparing a test sample, namely taking a proper amount of simethicone emulsion, precisely weighing, diluting, and filtering to obtain a test sample solution;
preparing reference, namely taking a proper amount of sorbic acid reference, precisely weighing, and diluting to obtain a reference solution;
detecting sorbic acid content in the sample solution by HPLC method.
Wherein, in the preparation of the test sample, a proper amount of simethicone emulsion is taken, precisely weighed, diluted and filtered to obtain the test sample solution:
the mixture is diluted by adding solvent to prepare 100mg of simethicone emulsion in each 1 ml.
Wherein, after the step of adding solvent and quantitatively diluting to prepare a solution containing 100mg of simethicone emulsion in each 1 ml:
shaking the solution evenly, filtering and taking filtrate.
Wherein, in the step of preparing the reference substance, taking a proper amount of sorbic acid reference substance, precisely weighing, and diluting to obtain a reference substance solution, the dilution process is as follows:
dissolving with solvent under ultrasonic wave, and quantitatively diluting to obtain solution containing sorbic acid 0.12mg per 1 ml.
Wherein, in the step of detecting the sorbic acid content in the sample solution by adopting an HPLC method:
a chromatographic column which takes octadecylsilane chemically bonded silica as a filler;
a mobile phase, taking sodium acetate buffer as a mobile phase A;
acetonitrile is used as a mobile phase B for gradient elution.
Wherein, in the step of taking sodium acetate buffer as mobile phase A, the preparation process of mobile phase A is as follows:
2.05g of anhydrous sodium acetate was taken, 1000ml of water was added to the anhydrous sodium acetate for dissolution, and the pH was adjusted to 4.5 with glacial acetic acid to obtain mobile phase A.
Wherein, in the step of gradient elution by taking acetonitrile as a mobile phase B:
the column temperature was 40℃and the flow rate was 0.8ml/min, the wavelength was 250nm, and the sample loading was 10. Mu.l.
The invention relates to a method for measuring sorbic acid in simethicone emulsion by an HPLC method, which comprises the steps of preparing a sample, taking a proper amount of simethicone emulsion, precisely weighing, diluting, and filtering to obtain a sample solution; preparing reference, namely taking a proper amount of sorbic acid reference, precisely weighing, and diluting to obtain a reference solution; detecting the content of the pear acid in the test solution by adopting an HPLC method; the method for measuring sorbic acid in simethicone emulsion by adopting the HPLC method can accurately detect the sorbic acid in the simethicone emulsion, has good separation degree from adjacent peaks, theoretical plate number and trailing factor symmetry factor and high response, is suitable for measuring the sorbic acid content in a multicomponent preparation, has strong specificity, high sensitivity, stability and reliability, can be used for measuring the sorbic acid content of the simethicone emulsion and controlling the quality, and provides a beneficial reference for the production process and medication safety.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of the steps of the method of determining sorbic acid in simethicone emulsion by HPLC according to the present invention.
FIG. 2 is a typical pattern of a blank solution of the present invention.
FIG. 3 is a typical spectrum of a blank stock and adjuvant solution of the present invention.
FIG. 4 is a typical pattern of a control solution of the present invention.
FIG. 5 is a typical pattern of a test solution of the present invention.
Detailed Description
Referring to fig. 1 to 5, fig. 1 is a flow chart of steps of a method for determining sorbic acid in simethicone emulsion by using an HPLC method, fig. 2 is a typical pattern of a blank solution, fig. 3 is a typical pattern of a blank raw and auxiliary material solution, fig. 4 is a typical pattern of a reference solution, and fig. 5 is a typical pattern of a sample solution.
The invention provides a method for measuring sorbic acid in simethicone emulsion by an HPLC method, which comprises the following steps:
s1: preparing a test sample, namely taking a proper amount of simethicone emulsion, precisely weighing, adding a solvent for quantitative dilution to prepare a solution containing 100mg of simethicone emulsion in each 1ml, shaking uniformly, and filtering to obtain a filtrate serving as a test sample solution;
s2: preparing reference, namely taking a proper amount of sorbic acid reference, precisely weighing, adding a solvent, performing ultrasonic dissolution, and quantitatively diluting to prepare a solution containing 0.12mg of sorbic acid in each 1ml, thereby obtaining a reference solution;
s3: detecting sorbic acid content in the sample solution by HPLC method.
In the embodiment, the test sample is prepared, a proper amount of simethicone emulsion is taken, precisely weighed, and added with solvent for quantitative dilution to prepare a solution containing 100mg of simethicone emulsion in each 1ml, and the solution is uniformly shaken, filtered and then the filtrate is taken as the test sample solution; preparing reference, namely taking a proper amount of sorbic acid reference, precisely weighing, adding a solvent, performing ultrasonic dissolution, and quantitatively diluting to prepare a solution containing 0.12mg of sorbic acid in each 1ml, thereby obtaining a reference solution; detecting the content of the pear acid in the test solution by adopting an HPLC method; the method for measuring sorbic acid in simethicone emulsion by adopting the HPLC method can accurately detect the sorbic acid in the simethicone emulsion, has good separation degree from adjacent peaks, theoretical plate number and trailing factor symmetry factor and high response, is suitable for measuring the sorbic acid content in a multicomponent preparation, has strong specificity, high sensitivity, stability and reliability, can be used for measuring the sorbic acid content of the simethicone emulsion and controlling the quality, and provides a beneficial reference for the production process and medication safety.
Wherein in the system applicability test:
blank solvent: sodium acetate buffer (2.05 g of anhydrous sodium acetate, 1000ml of water were added to dissolve, and the pH was adjusted to 4.5 with glacial acetic acid) -acetonitrile (60:40).
Preparing a reference substance solution: taking a proper amount of sorbic acid reference substance, precisely weighing, adding a solvent, carrying out ultrasonic dissolution and quantitatively diluting to prepare a solution containing about 0.12mg per 1 ml.
The system adaptability test measurement results are as follows:
| number of sample injections | Peak area | Retention time (min) | Number of theoretical plates |
| 1 | 6353.382 | 12.869 | 90483 |
| 2 | 6345.515 | 12.863 | 90652 |
| 3 | 6366.571 | 12.868 | 90042 |
| 4 | 6361.577 | 12.867 | 90056 |
| 5 | 6364.411 | 12.867 | 89964 |
| Average value of | 6358.291 | 12.867 | - |
| RSD(％) | 0.2 | 0.1 | - |
5 parts of reference solution spectrograms, RSD of sorbic acid peak area is less than 10.0%, RSD of retention time is less than 1.0%, theoretical plate number is more than 1000, and the requirements are met.
Wherein in the specificity test:
blank solvent: sodium acetate buffer (2.05 g of anhydrous sodium acetate, 1000ml of water were added to dissolve, and the pH was adjusted to 4.5 with glacial acetic acid) -acetonitrile (60:40).
Blank raw and auxiliary material solution: taking about 5g of blank emulsion (without sorbic acid), precisely weighing, placing into a 50ml measuring flask, adding solvent to dilute to scale, and filtering.
Control solution: taking a proper amount of sorbic acid reference substance, precisely weighing, adding a solvent, carrying out ultrasonic dissolution and quantitatively diluting to prepare a solution containing about 0.12mg per 1 ml.
Test solution: taking a proper amount of the product, precisely weighing, adding a solvent for quantitative dilution to prepare a solution containing about 100mg of the product in each 1ml, shaking uniformly, filtering, and taking filtrate as a test sample solution.
The specific test results are:
| solution name | The peak of the principal component |
| Blank solution | No interference |
| Blank raw and auxiliary material solution | No interference |
| Solution name | Main peak retention time (min) |
| Reference substance solution | 12.869 |
| Test solution | 12.855 |
The blank solution and the blank raw and auxiliary material solution have no interference to the determination of the sorbic acid content, the retention time of the main peak of the solution of the sample to be tested is consistent with the retention time of the main peak of the solution of the reference, and the requirements are met, so that the determination method has good specificity.
Wherein in the linear range test:
blank solvent: sodium acetate buffer (2.05 g of anhydrous sodium acetate, 1000ml of water were added to dissolve, and the pH was adjusted to 4.5 with glacial acetic acid) -acetonitrile (60:40).
Linear stock solution: taking about 48mg of sorbic acid reference substance, precisely weighing, placing into a 100ml measuring flask, adding a diluent, ultrasonically dissolving, and diluting to a scale to obtain a linear stock solution.
Linear test solution: the linear test solutions were prepared as follows
The linear test solution was formulated as:
sorbic acid is in the range of concentration 0.07367-0.14734ug/ml, and the linear regression equation is y=51476x+51.46; r is 0.9999, greater than 0.999; the Y-axis intercept is 51.46, less than 2% of the 100% response value, and the linearity is good.
Wherein in the precision test, a repeatability test is included:
blank solvent: sodium acetate buffer (2.05 g of anhydrous sodium acetate, 1000ml of water were added to dissolve, and the pH was adjusted to 4.5 with glacial acetic acid) -acetonitrile (60:40).
Control solution: taking a proper amount of sorbic acid reference substance, precisely weighing, adding a solvent, carrying out ultrasonic dissolution and quantitatively diluting to prepare a solution containing about 0.12mg per 1 ml. 2 parts were prepared in parallel.
Test solution: taking a proper amount of the product, precisely weighing, adding a solvent for quantitative dilution to prepare a solution containing about 100mg of the product in each 1ml, shaking uniformly, filtering, and taking filtrate as a test sample solution. 6 parts were prepared in parallel.
The repeatability test results were:
as a result of 6 times of measurement, the content of sorbic acid is in the range of 0.936-1.464 mg/ml, and the RSD value is 0.3% and less than 3.0%.
Wherein in the precision test, the precision test (intermediate precision) is included:
at the same laboratory, different times were measured by different analysts using different equipment.
The intermediate precision test results were:
the content RSD of sorbic acid in the two groups of measurement results of 12 times is 1.1 percent and less than 3.0 percent, which meets the requirements, and the measurement method has certain precision.
In accuracy testing:
blank solvent: sodium acetate buffer (2.05 g of anhydrous sodium acetate, 1000ml of water were added to dissolve, and the pH was adjusted to 4.5 with glacial acetic acid) -acetonitrile (60:40).
Control solution: taking a proper amount of sorbic acid reference substance, precisely weighing, adding a solvent, carrying out ultrasonic dissolution and quantitatively diluting to prepare a solution containing about 0.12mg per 1 ml.
Sorbic acid stock solution: taking about 48mg of sorbic acid reference substance, precisely weighing, placing into a 100ml measuring flask, adding diluent to dilute to scale, and shaking uniformly to obtain the final product.
Accuracy solution: weighing about 2g of blank emulsion (without sorbic acid), placing into a 20ml measuring flask, respectively precisely adding 3ml, 5ml and 6ml (corresponding to the concentration levels of 60%, 100% and 120% of the limit) of sorbic acid stock solution, adding solvent to dilute to scale, shaking uniformly, filtering, and taking filtrate. Each concentration level was formulated in the same way in 3 parts, 9 parts total.
The accuracy test results were:
the recovery rate of sorbic acid in 9 samples is between 90% and 108% at three concentration levels, and RSD is 0.3% and less than 3.0%, which proves that the measuring method has good accuracy.
In the solution stability test:
control solution: taking a proper amount of sorbic acid reference substance, precisely weighing, adding a solvent, carrying out ultrasonic dissolution and quantitatively diluting to prepare a solution containing about 0.12mg per 1 ml.
Test solution: taking a proper amount of the product, precisely weighing, adding a solvent for quantitative dilution to prepare a solution containing about 100mg of the product in each 1ml, shaking uniformly, filtering, and taking filtrate as a test sample solution.
The stability test result of the reference substance solution is as follows:
the test results of the stability of the test sample solution are as follows:
the relative deviation of peak areas of the control solution in 46 hours, the test solution in 43 hours and the peak area in 0 hour is between 98.0% and 102.0%, which shows that the stability of the control solution in 46 hours and the test solution in 43 hours is good.
In the durability test:
durability test parameters: the chromatographic condition variation parameters are shown in the following table.
The durability test parameters were:
blank solvent: sodium acetate buffer (2.05 g of anhydrous sodium acetate, 1000ml of water were added to dissolve, and the pH was adjusted to 4.5 with glacial acetic acid) -acetonitrile (60:40).
Control solution: taking a proper amount of sorbic acid reference substance, precisely weighing, adding a solvent, carrying out ultrasonic dissolution and quantitatively diluting to prepare a solution containing about 0.12mg per 1 ml.
Test solution: taking a proper amount of the product, precisely weighing, adding a solvent for quantitative dilution to prepare a solution containing about 100mg of the product in each 1ml, shaking uniformly, filtering, and taking filtrate as a test sample solution.
The durability test results were
The content of sorbic acid detected under each fluctuation chromatographic condition accords with the regulation, and the RSD content of 6 parts of the 4 parts of results of up-and-down fluctuation of the same parameter and the RSD content of 6 parts of the original 2 parts of results are less than or equal to 2.0 percent, which accords with the requirement, thus indicating that the measuring method has certain durability.
Further, in the step of detecting the sorbic acid content in the sample solution by using the HPLC method:
a chromatographic column which takes octadecylsilane chemically bonded silica as a filler;
a mobile phase, taking sodium acetate buffer as a mobile phase A;
acetonitrile is used as a mobile phase B for gradient elution.
Further, in the step of taking sodium acetate buffer as mobile phase A, the preparation process of mobile phase A is as follows:
2.05g of anhydrous sodium acetate was taken, 1000ml of water was added to the anhydrous sodium acetate for dissolution, and the pH was adjusted to 4.5 with glacial acetic acid to obtain mobile phase A.
Further, in the step of gradient elution with acetonitrile as mobile phase B:
the column temperature was 40℃and the flow rate was 0.8ml/min, the wavelength was 250nm, and the sample loading was 10. Mu.l.
In the embodiment, 2.05g of anhydrous sodium acetate is taken, 1000ml of water is added into the anhydrous sodium acetate for dissolution, and glacial acetic acid is used for regulating the pH value to 4.5, so that a mobile phase A is obtained; in the process of detecting the sorbic acid content in a sample solution by adopting an HPLC method, a chromatographic column is octadecylsilane chemically bonded silica gel as a filler; taking sodium acetate buffer solution as a mobile phase A and acetonitrile as a mobile phase B, and performing gradient elution; wherein in gradient elution, the column temperature is 40 ℃, the flow rate is 0.8ml/min, the wavelength is 250nm, and the sample injection amount is 10 μl.
The above disclosure is only a preferred embodiment of the present invention, and it should be understood that the scope of the invention is not limited thereto, and those skilled in the art will appreciate that all or part of the procedures described above can be performed according to the equivalent changes of the claims, and still fall within the scope of the present invention.
Claims (7)
1. A method for determining sorbic acid in simethicone emulsion by using an HPLC method, which is characterized by comprising the following steps:
preparing a test sample, namely taking a proper amount of simethicone emulsion, precisely weighing, diluting, and filtering to obtain a test sample solution;
preparing reference, namely taking a proper amount of sorbic acid reference, precisely weighing, and diluting to obtain a reference solution;
detecting sorbic acid content in the sample solution by HPLC method.
2. The method for determining sorbic acid in simethicone emulsion by using HPLC as claimed in claim 1, wherein in the steps of preparing the test sample, taking a proper amount of simethicone emulsion, precisely weighing, diluting and filtering to obtain the test sample solution:
the mixture is diluted by adding solvent to prepare 100mg of simethicone emulsion in each 1 ml.
3. A method for determining sorbic acid in simethicone emulsion by HPLC according to claim 2, characterised in that after the step of quantitative dilution with solvent to a solution containing 100mg of simethicone emulsion per 1 ml:
shaking the solution evenly, filtering and taking filtrate.
4. The method for determining sorbic acid in simethicone emulsion by using HPLC as claimed in claim 1, wherein in the step of preparing the reference, a proper amount of sorbic acid reference is taken, precisely weighed and diluted to obtain reference solution, the dilution process is as follows:
dissolving with solvent under ultrasonic wave, and quantitatively diluting to obtain solution containing sorbic acid 0.12mg per 1 ml.
5. The method for determining sorbic acid in simethicone emulsion by HPLC according to claim 1, wherein in the step of detecting sorbic acid content in the sample solution by HPLC:
a chromatographic column which takes octadecylsilane chemically bonded silica as a filler;
a mobile phase, taking sodium acetate buffer as a mobile phase A;
acetonitrile is used as a mobile phase B for gradient elution.
6. The method for determining sorbic acid in simethicone emulsion by HPLC according to claim 5, wherein in the step of using sodium acetate buffer as mobile phase A, the preparation process of mobile phase A is as follows:
2.05g of anhydrous sodium acetate was taken, 1000ml of water was added to the anhydrous sodium acetate for dissolution, and the pH was adjusted to 4.5 with glacial acetic acid to obtain mobile phase A.
7. The method for determining sorbic acid in simethicone emulsion by HPLC according to claim 5, wherein in the step of gradient elution with acetonitrile as mobile phase B:
the column temperature was 40℃and the flow rate was 0.8ml/min, the wavelength was 250nm, and the sample loading was 10. Mu.l.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310800219.9A CN116818946A (en) | 2023-07-03 | 2023-07-03 | Method for measuring sorbic acid in simethicone emulsion by HPLC (high Performance liquid chromatography) |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310800219.9A CN116818946A (en) | 2023-07-03 | 2023-07-03 | Method for measuring sorbic acid in simethicone emulsion by HPLC (high Performance liquid chromatography) |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116818946A true CN116818946A (en) | 2023-09-29 |
Family
ID=88115261
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310800219.9A Pending CN116818946A (en) | 2023-07-03 | 2023-07-03 | Method for measuring sorbic acid in simethicone emulsion by HPLC (high Performance liquid chromatography) |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116818946A (en) |
-
2023
- 2023-07-03 CN CN202310800219.9A patent/CN116818946A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| WO2021022876A1 (en) | Method for determining halogenated acid content in chloral hydrate or preparation thereof | |
| CN118010878A (en) | Determination method and application of impurities in sodium rabeprazole enteric-coated preparation | |
| CN111579706A (en) | Detection method of impurities in hydrolysis of brivaracetam | |
| CN110514759B (en) | Method for detecting azide in candesartan cilexetil | |
| CN114689737B (en) | Analysis method of S-o-chlorophenylglycine methyl tartrate related substances | |
| CN110954629A (en) | Control method for measuring content of furfuryl amine in furosemide | |
| CN111551645A (en) | Method for detecting hydroxychloroquine sulfate related substances and application thereof | |
| CN116818946A (en) | Method for measuring sorbic acid in simethicone emulsion by HPLC (high Performance liquid chromatography) | |
| CN110873767B (en) | Rapid detection method for dexlansoprazole synthetic intermediate and related substances thereof | |
| CN110082445B (en) | Method for simultaneously determining content of chlorhexidine gluconate and parachloroaniline | |
| CN110095554B (en) | Method for analyzing milrinone related substances by high performance liquid chromatography | |
| CN109765316B (en) | Method for detecting levetiracetam from medicine | |
| CN114518413A (en) | Method for measuring content of proline in captopril raw material medicine | |
| CN114200050B (en) | HPLC detection method for content of related substances in p-bromoanisole | |
| CN114994211B (en) | Kit for detecting catecholamine metabolite content in human urine and application thereof | |
| CN113866329B (en) | Method for detecting isocyanate potential genotoxic impurities in glimepiride tablets | |
| CN114354780B (en) | Method for detecting impurity content in ammonia bromine terro oral solution | |
| CN115372489B (en) | Detection method of tizanidine hydrochloride related substances | |
| CN115792047B (en) | Method for detecting related substances of tedizolid phosphate intermediate | |
| CN114414716B (en) | Detection method and application of triethylamine and N, N-diethylaniline in ceftazidime | |
| CN116930368B (en) | Detection method of settop alcohol isomer | |
| CN115236255B (en) | Method for detecting related substances of loxoprofen sodium | |
| CN112362778B (en) | Detection method of neratedlol intermediate related substances | |
| CN107091895B (en) | Method for separating and measuring related substances in riociguat raw material medicine by adopting HPLC (high performance liquid chromatography) | |
| CN118067860A (en) | Detection method of related substances in epalrestat tablet |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication |