CN111175385A - Irbesartan isomer testing method in irbesartan - Google Patents
Irbesartan isomer testing method in irbesartan Download PDFInfo
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Abstract
The invention relates to the field of organic chemistry and pharmaceutical analysis, in particular to a test method for separating and determining irbesartan isomers in irbesartan by high performance liquid chromatography, which mainly comprises the following steps: (1) determining chromatographic conditions through chromatographic columns, column temperature, detection wavelength and flow equality; (2) preparing blank solution, reference substance, test sample and other solutions; (3) the measuring method comprises precisely measuring blank solution, reference solution and sample solution, respectively, injecting into a liquid chromatograph, and recording chromatogram; (4) and (4) calculating. The detection method has high chromatographic peak separation degree and high system applicability, and meets the standards in the aspects of specificity, precision, quantitative limit, detection limit, accuracy, linearity, range, durability and the like.
Description
Technical Field
The invention relates to the field of organic chemistry and pharmaceutical analysis, in particular to a method for testing irbesartan isomerides.
Background
Irbesartan (irbesart) has the chemical name: 3- ((2'- (1H-tetrazol-5-yl) - [1,1' -biphenyl ] -4-yl) methyl) -2-butyl-1, 3-diazaspiro [4,4] non-1-en-4-one, developed by Sanofi and marketed in the United kingdom at the earliest in 1997. Irbesartan is an angiotensin II receptor (AT1 subtype) antagonist that blocks angiotensin II induced vasoconstriction and aldosterone secretion by selectively binding to the AT1 angiotensin II receptor. The medicine can be used for treating adult essential hypertension, and can also be used as part of antihypertensive drug treatment scheme, and can be used for treating nephropathy of adult patients with hypertension and type 2 diabetes.
At present, in the aspect of quality control of irbesartan raw material drugs, the irbesartan, an impurity I and other impurities in raw material drugs are mainly detected, and a potential process impurity, namely an irbesartan isomer exists in the irbesartan preparation process, and the irbesartan isomer has the chemical name: 1- ((2'- (1H-tetrazol-5-yl) - [1,1' -biphenyl ] -4-yl) methyl) -2-butyl-1, 3-diazaspiro [4,4] non-1-en-4-one.
At present, reports about irbesartan isomers are few, a preparation method of irbesartan isomers and irbesartan condensation product isomers as intermediates thereof are only disclosed in patent document CN106083826A, and a detection method about irbesartan isomers is not found.
Disclosure of Invention
The invention aims to provide a rapid and accurate method for testing irbesartan isomerides, which is implemented by high performance liquid chromatography and verified in the aspects of system adaptability, specificity, precision, quantitative limit, detection limit, durability and the like by referring to related contents of Chinese pharmacopoeia.
The method for testing the irbesartan isomeride mainly comprises the following steps:
(1) chromatographic conditions
The instrument comprises: a chromatographic column: octadecylsilane chemically bonded silica is used as a filling agent; the flow rate is 1.0 plus or minus 0.2 ml/min; detection wavelength: 220 +/-5 nm; sample introduction amount: 10 +/-2 mul; column temperature: 25 +/-2 ℃; operating time: 20 plus or minus 3 min; mobile phase: mixing the following raw materials in a phosphoric acid solution: the volume of acetonitrile is 65: 35;
the preparation method of the phosphoric acid solution comprises the steps of taking 5.5ml of 85 percent phosphoric acid, adding 950ml of water, and adjusting the pH value to 3.2 by triethylamine;
(2) preparing a solution: the diluent is methanol; the blank solution is a diluent; irbesartan isomer stock solution: the irbesartan isomer control substance has the concentration of 5 mug/ml; control solution: the irbesartan isomer control substance concentration is 0.5 mug/ml; test solution: the irbesartan test sample concentration is 0.5 mg/ml;
(3) measuring method and calculation formula
Injecting the blank solution, the reference solution and the sample solution into a liquid chromatograph, recording chromatogram, and obtaining the result%U/Rs)×(Cs/CU) X 100, wherein: rUPeak areas of irbesartan isomers in a test sample solution spectrum; rs-5 reference mean peak area of irbesartan isomer in reference solution chromatogram; cs-the concentration mg/ml of irbesartan isomer in the control solution; cUThe concentration of the test solution is mg/ml.
Further, the irbesartan isomer limits are as follows:
| name (R) | Acceptable Standard% | LOQ％ | LOD％ |
| Irbesartan isomer (RRT ≈ 0.4) | ≤0.1 | 0.03 | 0.01 |
Further, the method for testing irbesartan isomer in irbesartan also comprises a method verification before detection, and the chromatographic conditions verified by the method are consistent with those in the test method, and the specific contents are as follows:
(1) system adaptability
Chromatographic conditions are as follows: as described above.
Solution preparation: diluent, blank solution and control solution were as described above
The determination method comprises the following steps: and respectively injecting the blank solution and the reference solution into a liquid chromatograph, and recording the chromatogram.
(2) Specificity
Chromatographic conditions are as follows: as described above.
Solution preparation: besides the above-mentioned diluent, blank solution, stock solution, reference solution and sample solution, it also includes selective solution, and its preparation method is: taking an irbesartan sample of about 25mg, precisely weighing, placing in a 50ml volumetric flask, adding a proper amount of diluent for dissolution, precisely transferring 5.0ml of irbesartan isomer stock solution into the flask, adding the diluent for dilution to a scale, and shaking up uniformly. (concentration: irbesartan 0.5 mg/ml; irbesartan isomer 0.5. mu.g/ml)
The determination method comprises the following steps: and respectively injecting the blank solution, the reference solution, the test solution and the selective solution into a liquid chromatograph, and recording the chromatogram.
(3) Selectivity is
Chromatographic conditions are as follows: as described above.
Solution preparation: the diluent, blank solution, stock solution, control solution, test solution and optional solution are as described above.
The determination method comprises the following steps: and respectively injecting the reference solution, the test solution and the selective solution into a liquid chromatograph, and recording the chromatogram.
(4) Repeatability of
Chromatographic conditions are as follows: as described above.
Solution preparation: the diluent, blank solution, stock solution, control solution and test solution are as described above.
The determination method comprises the following steps: and respectively injecting the reference solution and the test solution into a liquid chromatograph, and recording the chromatogram.
(5) Quantitative and detection limits
Chromatographic conditions are as follows: as described above.
Solution preparation: the diluent, blank solution and stock solution are as above, and also include the following solutions,
test solution a: precisely transferring 6.0ml of irbesartan isomer stock solution, putting the irbesartan isomer stock solution into a 20ml volumetric flask, adding a diluent to dilute the irbesartan isomer stock solution to a scale, and shaking the solution uniformly.
LOQ solution: adjusting the dilution ratio according to the S/N value of the spectrum obtained by the test solution a until the S/N of the irbesartan isomer is approximately equal to 10; 6 parts of the solution is prepared by the same method.
LOD solution: precisely transferring 3.0ml of LOQ solution into a 10ml volumetric flask, adding diluent to dilute to the scale, and shaking up.
The determination method comprises the following steps: and respectively injecting the test solution a, the LOQ solution and the LOD solution into a liquid chromatograph, and recording the chromatogram.
(6) Stability of solution
Chromatographic conditions are as follows: as described above.
Solution preparation: the diluent, blank solution, control solution and test solution are as described above.
The determination method comprises the following steps: taking 3 parts of the reference solution and the sample solution respectively, standing at room temperature for 0 day, 1 day and 2 days, injecting into a liquid chromatograph, and recording chromatogram.
Further, the data acceptance criteria obtained in the method verification are as follows:
advantageous effects
According to the technical scheme, the detection method makes up the blank of the irbesartan isomer detection method in irbesartan, provides a quick and accurate irbesartan isomer detection method, and facilitates quality control of irbesartan raw material medicines. In addition, the detection method has high chromatographic peak separation degree and high system applicability, and meets the standards in specificity, precision, quantitative limit, detection limit, accuracy, linearity, range and durability.
Drawings
FIG. 1: a blank solution spectrogram;
FIG. 2: a system suitability solution profile;
FIG. 3: a spectrogram of the control solution;
FIG. 4: a spectrogram of the test solution;
FIG. 5: a selective solution spectrum;
FIG. 6: detecting a spectrogram through precision;
FIG. 7: detecting a spectrogram through quantitative limit;
FIG. 8: verifying a spectrogram of the detection limit;
FIG. 9: solution stability verification-the control solution is placed for 0 day spectrogram;
FIG. 10: solution stability verification-the control solution was left for 2 days spectrogram;
FIG. 11: verifying the stability of the solution, namely placing the test solution in a 0-day spectrogram;
FIG. 12: verifying the stability of the solution, namely placing the test solution for 2 days;
Detailed Description
The following examples illustrate the invention in detail to aid understanding, but are not intended to limit the invention.
Example 1
Examination of irbesartan isomers in irbesartan:
(1) chromatographic conditions
The instrument comprises the following steps: the high performance liquid chromatograph is provided with an ultraviolet detector, an electronic analytical balance and a pH meter
A chromatographic column: octadecylsilane chemically bonded silica is used as a filling agent; (e.g. thermo Acclaim 120C 18, 5 μm, 4.6X 150mm or equivalent performance columns);
flow rate: 1.0 ml/min; detection wavelength: 220 nm;
sample introduction amount: 10 mu l of the mixture; column temperature: 25 ℃;
operating time: 20 min;
mobile phase: adding a phosphoric acid solution (5.5 ml of 85% phosphoric acid, 950ml of water and adjusting the pH value to 3.2 by triethylamine): acetonitrile 65: 35 (V/V).
(2) Solution preparation:
diluting liquid: methanol;
blank solution: diluting the solution;
irbesartan isomer stock solution: taking irbesartan isomer reference substance of about 10mg, precisely weighing, placing in a 100ml volumetric flask, adding diluent to dissolve and dilute to a scale, and shaking up. Precisely transferring 5.0ml, placing in a 100ml volumetric flask, adding the diluent to dilute to the scale, and shaking up. (concentration: 5. mu.g/ml)
Control solution, i.e. control solution: precisely transferring 5.0ml of irbesartan isomer stock solution, putting the irbesartan isomer stock solution into a 50ml volumetric flask, adding diluent to dilute the irbesartan isomer stock solution to a scale, and shaking the irbesartan isomer stock solution uniformly. (concentration: 0.5. mu.g/ml)
Test solution, i.e. test solution: taking an irbesartan sample of about 25mg, precisely weighing, placing in a 50ml volumetric flask, adding a diluent to dissolve and dilute to a scale, and shaking uniformly. (concentration: 0.5mg/ml)
(3) Measurement method
After the system is stabilized, respectively injecting blank solution 1 needle, reference solution 5 needle and sample solution 1 needle into liquid chromatograph, recording chromatogram
(4) Formula for calculation
Results%U/Rs)×(Cs/CU)×100
Wherein: rU: peak areas of irbesartan isomers in a test solution spectrum;
rs: 5 average peak areas of irbesartan isomers in a reference substance solution spectrum;
cs: concentration of irbesartan isomer (mg/ml) in control solution;
CU: concentration of test solution (mg/ml).
(5) Limit of
Calculated from experimentally determined data, the irbesartan isomer limits are shown in the following table:
TABLE-1 Irbesartan isomeric limits
| Name (R) | Acceptable Standard% | LOQ％ | LOD％ |
| Irbesartan isomer (RRT ≈ 0.4) | ≤0.1 | 0.03 | 0.01 |
Example 2 system adaptability:
chromatographic conditions are as follows: as described in example 1.
Solution preparation: diluent, blank solution and control solution were as described in example 1
The determination method comprises the following steps: and after the system is stable, respectively injecting 1 needle of the blank solution and 5 needles of the reference solution into the liquid chromatograph, and recording the chromatogram.
And (3) measuring results: according to the measured spectrogram, the measurement results of the system suitability solution are shown in the following table:
TABLE-2 System suitability solution assay results
Example 3 specificity:
chromatographic conditions are as follows: as described in example 1.
Solution preparation: besides the diluent, the blank solution, the reference solution and the test solution in the above example 1, the solution also includes a selective solution, and the preparation method thereof is as follows: taking an irbesartan sample of about 25mg, precisely weighing, placing in a 50ml volumetric flask, adding a proper amount of diluent for dissolution, precisely transferring 5.0ml of irbesartan isomer stock solution into the flask, adding the diluent for dilution to a scale, and shaking up. (concentration: irbesartan 0.5 mg/ml; irbesartan isomer 0.5. mu.g/ml)
The determination method comprises the following steps: and after the system is stable, injecting a blank solution 1 needle, a reference solution 3 needle, a sample solution 1 needle and a selective solution 3 needle into the liquid chromatograph respectively, and recording the chromatogram.
And (3) measuring results: the results of the specificity test are shown in the following table:
TABLE-3 results of specificity test
Example 4 selectivity:
chromatographic conditions are as follows: as described in example 1.
Solution preparation: the control solution, test solution, and selection solution were as described in example 3.
The determination method comprises the following steps: and after the system is stable, respectively injecting 3 needles of the reference solution, 1 needle of the test solution and 3 needles of the selective solution into a liquid chromatograph, and recording the chromatogram.
And (3) measuring results: results of the specificity selectivity measurements are shown in the following table:
TABLE-4 results of specificity selectivity determination
Remarking: the area of the introduced peak is the area of the peak of the sample solution x the sample amount of the sample and the sample amount of the sample in the sample solution
Example 5 repeatability:
chromatographic conditions are as follows: as described in example 1.
Solution preparation: the diluent, blank solution, stock solution, control solution and test solution were as described in example 1.
The determination method comprises the following steps: and after the system is stabilized, respectively injecting 1 needle of the reference solution and 1 needle of each of 6 parts of the test solution into a liquid chromatograph, and recording the chromatogram.
And (3) measuring results: the results of the reproducibility measurements are shown in the following table,
TABLE-5 results of precision measurement
Note: the control solution referencing system was adapted for use with a first needle.
Example 6 limits of quantitation and detection
Chromatographic conditions are as follows: as described in example 1.
Solution preparation: dilutions, blank solutions, isomer stocks as described in example 1, also included the following solutions,
test solution a: precisely transferring 6.0ml of irbesartan isomer stock solution, putting the irbesartan isomer stock solution into a 20ml volumetric flask, adding a diluent to dilute the irbesartan isomer stock solution to a scale, and shaking the solution uniformly.
LOQ solution: adjusting the dilution ratio according to the S/N value of the spectrum obtained by the test solution a until the S/N of the irbesartan isomer is approximately equal to 10; 6 parts of the solution is prepared by the same method.
LOD solution: precisely transferring 3.0ml of LOQ solution into a 10ml volumetric flask, adding diluent to dilute to the scale, and shaking up.
The determination method comprises the following steps: and after the system is stabilized, injecting the sample solution a 1, 6 parts of LOQ solution and LOD solution into a liquid chromatograph, and recording the chromatogram. And (3) measuring results:
TABLE-6 results of measurement of quantitative limit and detection limit
TABLE-7 LOQ repeatability results
Example 7 solution stability
Chromatographic conditions are as follows: as described in example 1.
Solution preparation: the diluent, blank solution, control solution, and test solution were as described in example 1.
The determination method comprises the following steps: after the reference solution and the sample solution are placed at room temperature for 0 day, 1 day and 2 days, respectively injecting 1 needle of the reference solution for 0 day, 1 day and 2 days and 1 needle of the sample solution for 0 day, 1 day and 2 days into a liquid chromatograph when the system is stable, and recording the chromatogram.
And (3) measuring results:
TABLE-8 results of solution stability measurements
Claims (4)
1. A method for testing irbesartan isomers in irbesartan, comprising the steps of:
(1) chromatographic conditions
The instrument comprises: a chromatographic column: octadecylsilane chemically bonded silica is used as a filling agent; the flow rate is 1.0 plus or minus 0.2 ml/min; detection wavelength: 220 +/-5 nm; sample introduction amount: 10 +/-2 mul; column temperature: 25 +/-2 ℃; operating time: 20 plus or minus 3 min; mobile phase: mixing the following raw materials in a phosphoric acid solution: the volume of acetonitrile is 65: 35;
the preparation method of the phosphoric acid solution comprises the steps of taking 5.5ml of 85 percent phosphoric acid, adding 950ml of water, and adjusting the pH value to 3.2 by triethylamine;
(2) preparing a solution: the diluent is methanol; the blank solution is a diluent; irbesartan isomer stock solution: the irbesartan isomer control substance has the concentration of 5 mug/ml; control solution: the irbesartan isomer control substance concentration is 0.5 mug/ml; test solution: the irbesartan test sample concentration is 0.5 mg/ml;
(3) measuring method and calculation formula
Injecting the blank solution, the reference solution and the sample solution into a liquid chromatograph, recording the chromatogram, and obtaining the result% = (R)U/Rs) ×(Cs/CU) X 100, wherein: rUPeak areas of irbesartan isomers in a test sample solution spectrum; rs-5 reference mean peak area of irbesartan isomer in reference solution chromatogram; cs-the concentration mg/ml of irbesartan isomer in the control solution; cUThe concentration of the test solution is mg/ml.
2. The method for testing irbesartan isomers in irbesartan according to claim 1, wherein the irbesartan isomer limit is:
。
3. The method for testing irbesartan isomers in irbesartan according to claim 1, wherein the method for testing irbesartan further comprises a method for verifying that the chromatographic conditions verified by the method are consistent with those of the method for testing, and the method comprises the following specific steps:
(1) system adaptability
Chromatographic conditions are as follows: as described above;
solution preparation: the diluent, blank solution and control solution are as described in claim 1;
the determination method comprises the following steps: respectively injecting the blank solution and the reference solution into a liquid chromatograph, and recording a chromatogram;
(2) specificity
Chromatographic conditions are as follows: as claimed in claim 1;
solution preparation: besides the diluent, the blank solution, the stock solution, the reference solution and the test solution, the selective solution also comprises a selective solution, wherein the irbesartan concentration is 0.5mg/ml, and the irbesartan isomer concentration is 0.5 mu g/ml;
the determination method comprises the following steps: injecting the blank solution, the reference solution, the test solution and the selective solution into a liquid chromatograph, and recording the chromatogram;
(3) selectivity is
Chromatographic conditions are as follows: as claimed in claim 1;
solution preparation: diluting solution, blank solution, stock solution, reference solution, sample solution and optional solution as described in (2) specificity step;
the determination method comprises the following steps: injecting the reference solution, the test solution and the selective solution into a liquid chromatograph, and recording the chromatogram;
(4) repeatability of
Chromatographic conditions are as follows: as claimed in claim 1;
solution preparation: diluting solution, blank solution, stock solution, reference solution, and sample solution as described in (2);
the determination method comprises the following steps: injecting the reference solution and the test solution into a liquid chromatograph, and recording chromatograms;
(5) quantitative and detection limits
Chromatographic conditions are as follows: as claimed in claim 1;
solution preparation: the diluent, blank solution and stock solution as described in (2) the specific steps further include the following solutions:
test solution a: precisely transferring 6.0ml of irbesartan isomer stock solution, placing the irbesartan isomer stock solution into a 20ml volumetric flask, adding a diluent to dilute the irbesartan isomer stock solution to a scale, and shaking the solution uniformly;
LOQ solution: adjusting the dilution ratio according to the S/N value of the spectrum obtained by the test solution a until the S/N of the irbesartan isomer is approximately equal to 10; preparing 6 parts of the solution by the same method;
LOD solution: precisely transferring 3.0ml of LOQ solution into a 10ml volumetric flask, adding diluent to dilute to a scale, and shaking up;
the determination method comprises the following steps: respectively injecting the test solution a, the LOQ solution and the LOD solution into a liquid chromatograph, and recording the chromatogram;
(6) stability of solution
Chromatographic conditions are as follows: as claimed in claim 1;
solution preparation: diluting solution, blank solution, reference solution, and sample solution as described in (2);
the determination method comprises the following steps: taking 3 parts of the reference solution and the sample solution respectively, standing at room temperature for 0 day, 1 day and 2 days, injecting into a liquid chromatograph, and recording chromatogram.
4. The method for testing irbesartan isomers in irbesartan according to claim 1, wherein the data obtained in the method verification are accepted according to the following standards and the test results are as follows:
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