CN113325118B - Method for measuring sodium content in parecoxib sodium - Google Patents
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- 229960003925 parecoxib sodium Drugs 0.000 title claims abstract description 77
- ICJGKYTXBRDUMV-UHFFFAOYSA-N trichloro(6-trichlorosilylhexyl)silane Chemical compound Cl[Si](Cl)(Cl)CCCCCC[Si](Cl)(Cl)Cl ICJGKYTXBRDUMV-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 49
- 239000011734 sodium Substances 0.000 title claims abstract description 49
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 38
- 229910001415 sodium ion Inorganic materials 0.000 claims abstract description 58
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000007864 aqueous solution Substances 0.000 claims abstract description 20
- 229940098779 methanesulfonic acid Drugs 0.000 claims abstract description 17
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 16
- 239000003480 eluent Substances 0.000 claims abstract description 9
- 239000012086 standard solution Substances 0.000 claims description 44
- 239000000243 solution Substances 0.000 claims description 22
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 230000014759 maintenance of location Effects 0.000 claims description 14
- 238000005303 weighing Methods 0.000 claims description 9
- 238000004255 ion exchange chromatography Methods 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 7
- 238000010812 external standard method Methods 0.000 claims description 6
- 239000012528 membrane Substances 0.000 claims description 6
- 238000005341 cation exchange Methods 0.000 claims description 4
- 239000012085 test solution Substances 0.000 claims description 4
- HNSDLXPSAYFUHK-UHFFFAOYSA-N 1,4-bis(2-ethylhexyl) sulfosuccinate Chemical compound CCCCC(CC)COC(=O)CC(S(O)(=O)=O)C(=O)OCC(CC)CCCC HNSDLXPSAYFUHK-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims 1
- -1 ammonium ions Chemical class 0.000 abstract description 11
- 238000010828 elution Methods 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 3
- 238000004458 analytical method Methods 0.000 abstract description 2
- 150000002500 ions Chemical class 0.000 description 12
- 238000012360 testing method Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 7
- 238000011084 recovery Methods 0.000 description 7
- 238000010998 test method Methods 0.000 description 5
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 230000002980 postoperative effect Effects 0.000 description 4
- 238000005070 sampling Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 230000000202 analgesic effect Effects 0.000 description 2
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 238000012417 linear regression Methods 0.000 description 2
- BQJCRHHNABKAKU-KBQPJGBKSA-N morphine Chemical compound O([C@H]1[C@H](C=C[C@H]23)O)C4=C5[C@@]12CCN(C)[C@@H]3CC5=CC=C4O BQJCRHHNABKAKU-KBQPJGBKSA-N 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 208000002193 Pain Diseases 0.000 description 1
- 208000005298 acute pain Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 229940111134 coxibs Drugs 0.000 description 1
- 239000003255 cyclooxygenase 2 inhibitor Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000001990 intravenous administration Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000012982 microporous membrane Substances 0.000 description 1
- 229960005181 morphine Drugs 0.000 description 1
- 230000000399 orthopedic effect Effects 0.000 description 1
- 229960004662 parecoxib Drugs 0.000 description 1
- TZRHLKRLEZJVIJ-UHFFFAOYSA-N parecoxib Chemical compound C1=CC(S(=O)(=O)NC(=O)CC)=CC=C1C1=C(C)ON=C1C1=CC=CC=C1 TZRHLKRLEZJVIJ-UHFFFAOYSA-N 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000012088 reference solution Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000012487 rinsing solution Substances 0.000 description 1
- 150000003385 sodium Chemical class 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 238000001356 surgical procedure Methods 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
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- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- 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
- G01N30/86—Signal analysis
- G01N30/8624—Detection of slopes or peaks; baseline correction
- G01N30/8631—Peaks
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Pathology (AREA)
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Abstract
The invention provides a method for measuring sodium content in parecoxib sodium, which belongs to the technical field of analysis. According to the parecoxib sodium elution method, the mixed aqueous solution of methane sulfonic acid and nitric acid is used as the eluent to elute the parecoxib sodium, so that the base lines of sodium ions and ammonium ions contained in the parecoxib sodium can be well separated, the formed peak is good, the solvent peak does not interfere with the ammonium ions, the sodium content in the parecoxib sodium can be accurately detected, and the parecoxib sodium elution method has high specificity.
Description
Technical Field
The invention relates to a method for measuring sodium content, in particular to a method for measuring sodium content in parecoxib sodium.
Background
The Parecoxib Sodium (Parecoxib Sodium) is a COX-2 inhibitor for injection, can be used for treating postoperative moderate and severe acute pain, and the clinical curative effect of the Parecoxib Sodium is proved in postoperative analgesic treatment of various surgeries such as stomatology, gynecology, orthopedics and the like, and the postoperative intravenous administration of the Parecoxib Sodium can reduce the dosage of morphine and improve the postoperative analgesic quality.
Parecoxib sodium can be produced in large scale at home and abroad, and is generated by reacting parecoxib with sodium hydroxide, the sodium content in the parecoxib sodium can be accurately measured, and whether the parecoxib sodium is generated can be more accurately judged, so that the accuracy of measuring the sodium content in the parecoxib sodium is related to the quality of the finally obtained medicine. According to the report of the document "progress of research method for measuring trace elements by atomic absorption spectrometry", the atomic absorption spectrometry has a narrow linear range, is not suitable for analyzing elements with high concentration, and has the defects that the sampling amount is small, the variation of the sampling amount and the position in an injection pipe causes deviation, and the like. The ion chromatography developed by the invention has the advantages of wide linear range, good precision, simplicity, rapidness and high efficiency, and can well control the quality of the medicine.
Disclosure of Invention
In order to solve the problems, the invention provides a method for determining the sodium content in parecoxib sodium.
In order to realize the purpose, the technical scheme adopted by the invention is as follows:
a method for determining the sodium content in parecoxib sodium comprises the following steps:
accurately weighing sodium element standard solution and ammonium ion standard solution with different volumes respectively, and adding water to prepare standard solution;
accurately weighing parecoxib sodium, and adding water to prepare a solution to be detected;
taking a mixed aqueous solution of methane sulfonic acid and nitric acid as an eluent, taking a standard solution for ion chromatography determination, and determining the retention time of sodium ions and the peak area of the sodium ions in the standard solution;
taking a mixed aqueous solution of methanesulfonic acid and nitric acid as an eluent, taking a solution to be detected for ion chromatographic determination, determining the peak area of sodium ions in the solution to be detected according to the retention time of the sodium ions, and then calculating the sodium content in parecoxib sodium according to a formula I by an external standard method, wherein the formula I is as follows:
wherein: a. The R Is the peak area of sodium ions in the standard solution;
C R is the concentration of sodium ions in the standard solution, and the unit is mu g/mL;
A S the peak area of sodium ions in the liquid to be detected is shown;
C S in the liquid to be testedThe concentration of parecoxib sodium is in mg/mL.
Further, the mixed aqueous solution of the methanesulfonic acid and the nitric acid is prepared by uniformly mixing a 25mmol/L methanesulfonic acid aqueous solution and a 2.5mmol/L nitric acid aqueous solution in a volume ratio of 8.
Further, the concentration of parecoxib sodium in the solution to be detected is 0.24-0.26 mg/mL.
Further, the chromatographic conditions of the ion chromatograph are as follows: the sample introduction volume is 50 mu L, the flow rate is 1.1-1.3 mL/min, and the column temperature is 28-32 ℃.
Further, the chromatographic column of the ion chromatograph is a cation exchange column.
Further, the cation exchange column is Thermo Dionex IonPac TM CS12A RFIC TM 。
Furthermore, before the standard solution and the solution to be detected are loaded, a water system filter membrane is used for filtering, and then the sample solution passes through an RP column (the sample solution is filtered by the RP column, so that organic impurities can be removed).
Further, the aperture of the filtered water-based filter membrane is 0.22 μm.
Furthermore, the concentration of sodium ions in the standard solution is 14-16 mug/mL, and the concentration of ammonium ions in the standard solution is 1-1.5 mug/mL.
The method for determining the sodium content in parecoxib sodium has the beneficial effects that:
the method adopts the ion chromatography to detect the sodium content in the parecoxib sodium, has high precision and good repeatability, and can well control the quality of the medicament;
according to the parecoxib sodium elution method, the mixed aqueous solution of methane sulfonic acid and nitric acid is used as the eluent to elute the parecoxib sodium, so that the base lines of sodium ions and ammonium ions contained in the parecoxib sodium can be well separated, the formed peak is good, the solvent peak does not interfere with the ammonium ions, the sodium content in the parecoxib sodium can be accurately detected, and the parecoxib sodium elution method has high specificity.
Drawings
FIG. 1 is an ion chromatogram of a solution to be measured in example 1 of the present invention;
FIG. 2 is an ion chromatogram of a standard solution in comparative example 1 of Experimental example 5 of the present invention;
FIG. 3 is an ion chromatogram of a standard solution in comparative example 2 of Experimental example 5 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, however, the present invention may be practiced otherwise than as specifically described herein, and it will be appreciated by those skilled in the art that the present invention may be practiced without departing from the spirit and scope of the present invention and that the present invention is not limited by the specific embodiments disclosed below.
In the following examples, all reagents were commercially available unless otherwise specified, and the test methods were carried out according to the conventional test methods.
The instrument comprises: ion chromatograph (model: AQUION, brand: thermo);
an electronic balance (model: XS105, brand: mettler-Torlo);
reagent: methane sulfonic acid (content: 98%, hebei Bailingwei);
standard solution of sodium element (1000. Mu.g/mL, batch number: 207009-7, national center for analysis and test of nonferrous metals and electronic materials);
ammonium ion standard solution (1000. Mu.g/mL, batch number: BCBV9772, SIGMA-ALDRICH).
Example 1 method for determining sodium content in parecoxib sodium
The embodiment is a method for measuring the sodium content in parecoxib sodium, and the specific preparation process comprises the following steps in sequence:
1) Preparing standard solution
Accurately transferring 5mL of sodium element standard solution (the concentration of sodium element is 1000 mug/mL) into a 10mL volumetric flask, adding water to a constant volume, shaking up to obtain sodium element intermediate solution;
accurately transferring 3mL of sodium element intermediate solution and 1mL of ammonium ion standard solution (the ammonium ion concentration is 1000 mu g/mL), adding into a 100mL volumetric flask, adding water to constant volume until the volume is scaled, shaking up, and passing through a 0.2-meter flaskFiltering with 2 μm microporous membrane to obtain standard solution with sodium ion concentration of 15 μ g/mL (as C) R ) And the ammonium ion concentration was 1. Mu.g/mL.
2) Preparing the solution to be tested
Accurately weighing 25.81mg of parecoxib sodium (batch: T201201), adding into a 100mL volumetric flask, adding water to dilute until the scale is uniform, filtering with a 0.22 μm water-based filter membrane, and passing through an RP column to obtain a solution to be tested, wherein the concentration of parecoxib sodium is 0.25mg/mL (namely C) S )。
3) Method for measuring content of sodium ions in parecoxib sodium by external standard method
Taking 800mL of 25mmol/L methane sulfonic acid aqueous solution and 100mL of 2.5mmol/L nitric acid aqueous solution, and uniformly stirring to obtain a mixed aqueous solution of methane sulfonic acid and nitric acid;
the chromatographic conditions were set as follows: chromatography column (Thermo Dionex IonPac) TM CS12A RFIC TM 250mm multiplied by 5 mm), the sample injection volume is 50 mu L, the flow rate is 1.2mL/min, and the column temperature is 30 ℃;
taking a mixed aqueous solution of methanesulfonic acid and nitric acid as an eluent, sampling a standard solution in an ion chromatograph, and determining the retention time (3.8-4.6 min) of sodium ions and the peak area (A) of the sodium ions in the standard solution R ＝277.303)；
Taking a mixed aqueous solution of methanesulfonic acid and nitric acid as a leacheate, sampling a to-be-detected solution on an ion chromatograph to obtain an ion chromatogram of the to-be-detected solution, and determining the peak area (namely A) of sodium ions in the to-be-detected solution in the ion chromatogram of the to-be-detected solution according to the retention time (3.8-4.4 min) of the sodium ions, referring to fig. 1 S = 274.185), and then calculating the content of sodium ions in parecoxib sodium according to a formula I by an external standard method; the specific formula I is as follows:
wherein: a. The R Is the peak area of sodium ions in the standard solution;
C R the concentration of sodium ions in the standard solution is expressed in the unit of mu g/mL;
A S the peak area of sodium ions in the liquid to be detected is shown;
C S the concentration of parecoxib sodium in the solution to be detected is in mg/mL.
This time, the sodium ion content in parecoxib sodium was calculated to be 5.75% (note that the sodium ion content in parecoxib sodium was calculated for the first time).
Then, by the same method, the parecoxib sodium (batch: T201201) is measured again, and the content of the sodium ions in the parecoxib sodium is calculated to be 5.78% (recorded as the content of the sodium ions in the parecoxib sodium is calculated for the second time)
By calculating the average value of the sodium ion content in the parecoxib sodium twice, the sodium ion content in the parecoxib sodium is finally obtained to be 5.77%.
Example 2 to 6A method for measuring the sodium content in parecoxib sodium
Examples 2 to 6 are methods for determining the sodium content in parecoxib sodium, and the procedure is substantially the same as in example 1, except for the differences in the process parameters, as detailed in table 1:
TABLE 1 summary of the process parameters of examples 2 to 6
The contents of the other portions of examples 2 to 6 are the same as those of example 1.
Experimental example 1 precision test
Taking the standard solution in the example 1, repeating the sample injection for 6 times according to the method in the example 1, recording the retention time and the peak area of the sodium ions, and respectively calculating the relative standard deviation of the retention time and the relative standard deviation of the peak area, which are shown in the following table:
TABLE 2 results of precision tests
As can be seen from table 2, the relative standard deviation of the retention time of the sodium ions is 0.04%, the relative standard deviation of the peak area is 0.23%, and the relative deviation is small, which indicates that the method for determining the sodium content in parecoxib sodium in example 1 of the present invention has good precision and strong feasibility.
The precision of the methods of examples 2 to 6 was examined according to the same precision test method, wherein the relative standard deviation of the retention time of sodium ions of the standard solution and the chromatographic conditions in example 2 was 0.05%, and the relative standard deviation of the peak area was 0.26%; the relative standard deviation of the standard solution in example 3 and the sodium ion retention time corresponding to the chromatographic conditions was 0.07%, and the relative standard deviation of the peak area was 0.29%; the relative standard deviation of the standard solution in example 4 to the retention time of sodium ions corresponding to the chromatographic conditions was 0.06%, and the relative standard deviation of the peak area was 0.24%; the relative standard deviation of the standard solution in example 5 and the retention time of sodium ions corresponding to the chromatographic conditions was 0.04%, and the relative standard deviation of the peak area was 0.28%; the standard solution in example 6 had a relative standard deviation of 0.06% of the retention time of sodium ions and a relative standard deviation of 0.30% of the peak area corresponding to the chromatographic conditions. Therefore, the method for measuring the sodium content in the parecoxib sodium in the embodiments 2 to 6 has good precision and strong feasibility.
In conclusion, the method for determining the sodium content in the parecoxib sodium has good precision and strong feasibility.
Experimental example 2 Linear test
Respectively taking sodium element standard solution and adding water in a preset concentration range of 3-22.5 mu g/mL to prepare a series of sodium element standard reference solutions with sodium ion concentrations of 3 mu g/mL, 6 mu g/mL, 7.5 mu g/mL, 12 mu g/mL, 15 mu g/mL and 22.5 mu g/mL;
according to the chromatographic conditions in example 1, the samples are respectively loaded on an ion chromatograph, the peak areas and the corresponding concentrations thereof are recorded and plotted, and a linear regression equation and a regression coefficient are calculated, wherein the obtained linear regression equation is y =18.426x-0.6718, and the correlation coefficient is 1.000.
Because the concentration range of sodium ions is 3-22.5 mug/mL, under the chromatographic conditions of the embodiment 1, the peak area in the obtained chromatogram is in a linear relation with the concentration, and therefore, the sodium content in the parecoxib sodium calculated by the external standard method in the embodiment 1 has accuracy.
According to the same linear test method, linear relations between peak areas and concentrations under the chromatographic conditions in examples 2 to 6 are respectively examined, and the linear relations between peak areas and concentrations in chromatograms under the chromatographic conditions in examples 2 to 6 are confirmed, so that the sodium content in parecoxib sodium calculated by the external standard method in examples 2 to 6 is also accurate.
Experimental example 3 repeatability test
Accurately weighing 6 parts of parecoxib sodium 25mg respectively, adding the parecoxib sodium into a 100mL volumetric flask, adding water to dilute the parecoxib sodium until the scales are uniformly shaken, filtering the parecoxib sodium by a 0.22 mu m microporous filter membrane, taking the subsequent filtrate, and passing the subsequent filtrate through an RP column to prepare 6 parts of parallel test solutions which are respectively numbered as 01-06, wherein the concentration of the parecoxib sodium is 0.25mg/mL;
according to the methods in the embodiments 1 to 6, 6 parts of parallel test solutions are taken for ion chromatography determination, and the sodium content in parecoxib sodium corresponding to the 6 parts of parallel test solutions is calculated, and the specific results are shown in the following table:
TABLE 3 summary of test results
As can be seen from Table 3, the methods for determining the sodium content in parecoxib sodium in the embodiments 1 to 6 have better repeatability.
Experimental example 4 recovery test
Precisely measuring 5mL of sodium element standard solution, adding the sodium element standard solution into a 10mL volumetric flask, adding water to a constant volume, shaking up to a scale, and taking the solution as a stock solution.
Weighing parecoxib sodium (weighing 0.75mg of sodium ion content), adding the parecoxib sodium into a 100mL volumetric flask, weighing and counting the amount of sodium ions in parecoxib sodium actually added into the volumetric flask again (namely, the sodium ion bottom amount), adding the storage liquid according to 80%, 100% and 120% of the sodium ion bottom amount respectively [ wherein 80%, 100% or 120% is respectively equal to the sum of the sodium ion bottom amount and the amount of sodium element correspondingly added into the storage liquid ], dividing the sum by 2 times of the sodium ion bottom amount, namely 80% = (the amount of sodium element added into the storage liquid when the sodium ion bottom amount is plus 80% /'s the amount of sodium element added into the storage liquid)/(the sodium ion bottom amount × 2) ], adding water to dilute the scales, and then calculating the recovery rate of sodium element according to the chromatographic conditions and the calculation method in the example 1, wherein the result table is shown below.
TABLE 4 recovery test results
As can be seen from table 4, the method in example 1 of the present invention has a high recovery rate, and can accurately determine the sodium content in parecoxib sodium.
According to the same recovery rate test method, the recovery rates of the methods in the examples 2 to 6 are respectively examined, and the results prove that the recovery rates are very high under the chromatographic conditions of the examples 2 to 6, and the sodium content in parecoxib sodium can be accurately measured in the examples 2 to 6.
Experimental example 5 comparative experiment
Comparative examples 1 and 2 are comparative tests of the method for determining the sodium content in parecoxib sodium in example 1, differing only in that:
in comparative example 1, 2.5mmol/L nitric acid aqueous solution was used as a rinsing solution, and the standard solution and the chromatographic conditions were the same as in example 1; referring to fig. 2, the spectrum obtained after the standard solution is loaded shows that the peak patterns of sodium ions and ammonium ions are poor, wherein the theoretical plate number of the sodium ions is 3703, the theoretical plate number of the ammonium ions is 3322, the separation effect is poor, and the accuracy of the sodium ion content determination is affected under the condition of containing the ammonium ions.
In comparative example 2, a 25mmol/L aqueous solution of methanesulfonic acid was used as a rinse, and the standard solution and chromatographic conditions were the same as in example 1; referring to fig. 3, the spectrum obtained after the standard solution is loaded can show that sodium ions and ammonium ions can not be well separated, the separation degree is less than 1.5, the baseline separation is not achieved, and the content of the sodium ions can not be measured.
In conclusion, the parecoxib sodium is eluted by taking the mixed aqueous solution of the methanesulfonic acid and the nitric acid as the eluent, so that the base lines of sodium ions and ammonium ions contained in the parecoxib sodium can be well separated, the formed peak is good, the solvent peak does not interfere with the ammonium ions, the sodium content in the parecoxib sodium can be accurately detected, and the parecoxib sodium eluent has high specificity.
It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (5)
1. A method for determining the sodium content of parecoxib sodium, comprising the steps of:
accurately weighing sodium element standard solution and ammonium ion standard solution with different volumes respectively, and adding water to prepare standard solution;
accurately weighing parecoxib sodium, and adding water to prepare a solution to be detected;
taking a mixed aqueous solution of methanesulfonic acid and nitric acid as an eluent, taking a standard solution for ion chromatography determination, and determining the retention time of sodium ions and the peak area of the sodium ions in the standard solution;
taking a mixed aqueous solution of methanesulfonic acid and nitric acid as an eluent, taking a solution to be detected, performing ion chromatography determination, determining the peak area of sodium ions in the solution to be detected according to the retention time of the sodium ions, and then calculating according to a formula I by an external standard method to obtain the sodium content in parecoxib sodium, wherein the formula I is as follows:
content of sodium ions in parecoxib sodium =
-formula I;
wherein: a. The R Is the peak area of sodium ions in the standard solution;
C R the concentration of sodium ions in the standard solution is expressed in the unit of mu g/mL;
A S the peak area of sodium ions in the liquid to be detected is shown;
C S the concentration of parecoxib sodium in the solution to be detected is mg/mL;
the mixed aqueous solution of the methanesulfonic acid and the nitric acid is prepared by uniformly mixing 25mmol/L methanesulfonic acid aqueous solution and 2.5mmol/L nitric acid aqueous solution in a volume ratio of 8:1.8 to 2.3;
the chromatographic conditions of the ion chromatography are as follows: the sample introduction volume is 50 mu L, the flow rate is 1.1 to 1.3mL/min, and the column temperature is 28 to 32 ℃;
the chromatographic column of the ion chromatography is a cation exchange column;
the cation exchange column is Thermo Dionex IonPac TM CS12A RFIC TM 。
2. The method for determining the sodium content in parecoxib sodium according to claim 1, wherein the concentration of parecoxib sodium in the solution to be determined is 0.24-0.26mg/mL.
3. The method of claim 1, wherein the standard solution and the test solution are filtered through a water-based membrane before being applied to the RP column.
4. The method for determining the sodium content of parecoxib sodium according to claim 3, wherein the pore size of the aqueous filter membrane is 0.22 μm.
5. The method for determining the sodium content in parecoxib sodium according to claim 1 or 4, wherein the sodium ion concentration and the ammonium ion concentration in the standard solution are respectively 14 to 16 μ g/mL and 1 to 1.5 μ g/mL.
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