CN113687016B - Method for detecting chloride ion content in cyclobenzaprine hydrochloride - Google Patents
Method for detecting chloride ion content in cyclobenzaprine hydrochloride Download PDFInfo
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- CN113687016B CN113687016B CN202111055949.8A CN202111055949A CN113687016B CN 113687016 B CN113687016 B CN 113687016B CN 202111055949 A CN202111055949 A CN 202111055949A CN 113687016 B CN113687016 B CN 113687016B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
- G01N31/162—Determining the equivalent point by means of a discontinuity
- G01N31/164—Determining the equivalent point by means of a discontinuity by electrical or electrochemical means
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
Abstract
The invention provides a method for detecting the content of chloride ions in cyclobenzaprine hydrochloride. The method for detecting the chloride ion content in cyclobenzaprine hydrochloride comprises the following steps: (1) sample preparation: mixing cyclobenzaprine hydrochloride, nitric acid, a nonionic surfactant and water to obtain a sample solution; (2) potentiometric titration analysis: and titrating the sample solution by adopting silver nitrate solution, and calculating to obtain the chloride ion content. The invention adopts a potentiometric titration method to analyze the sample, and determines the titration endpoint through the change of potential. The invention has the advantages of high accuracy, quick analysis, strong anti-interference performance and high sensitivity.
Description
Technical Field
The invention belongs to the technical field of chemical analysis, and particularly relates to a method for detecting the content of chloride ions in cyclobenzaprine hydrochloride.
Background
Chloride ion is a common inorganic anion, but certain harm can be generated when the concentration is too high, so that the control of the content of the chloride ion is an important item in the quality control of bulk drugs. The common detection methods of chloride ions are four: (1) silver nitrate titration; (2) mercury nitrate titration; (3) potentiometric titration; (4) ion chromatography. The method (3) is suitable for measuring colored and turbid liquid, wherein a composite silver ring intelligent electrode is used as an electrode, and a silver nitrate standard solution is used as a titrant. In the titration process, the concentration of chloride ions is changed continuously along with the continuous addition of the titrant, the potential of the electrode is changed correspondingly, and the concentration of ions is suddenly changed near a stoichiometric point to cause the potential of the electrode to be suddenly changed, so that the endpoint is determined.
CN112986163a discloses a chloride ion concentration detection method based on spectral analysis, which belongs to the technical field of chloride ion detection. The method is characterized in that microemulsion consisting of n-butanol, triton, cyclohexane and deionized water is used as a high-stability detection reagent which is formed by nitric acid reagent and silver nitrate solution, and a silver chloride suspension formed by a chloride ion solution to be detected and the high-stability detection reagent has special light absorption characteristics. The method is not suitable for measuring the chloride ion content in cyclobenzaprine hydrochloride, and is realized by utilizing a relation model of the chloride ion content and absorbance in suspension.
CN109212002a discloses a method for detecting chloride ions in nicotinic acid by using a potentiometric titration method, which comprises the following steps: weighing a nicotinic acid sample into a beaker, adding deionized water, dissolving in ultrasonic, filtering with medium-speed qualitative filter paper into a volumetric flask, and shaking to a constant volume; transferring 50mL of sample liquid from a volumetric flask to a beaker, adding 0.5mL of nitric acid solution, placing the solution into a rotor and fixing the solution on a magnetic stirrer, adjusting an acidometer to a potential level, taking a silver electrode as an indicating electrode, a double-salt bridge type saturated calomel electrode as a reference electrode, titrating with a silver nitrate standard solution, recording a consumed volume V and a potential value E every 0.05-0.1mL, and ending the titration when the potential is indicated to 350; the method has the problem that sediment adheres to the electrode during titration, thereby causing interference to measurement.
CN112557583a discloses a method for determining the chloride ion content in the admixture by potentiometric titration. The method comprises the following steps: mixing 1-5g of additive with 5-10mL of nitric acid solution, 100-300mL of deionized water and 0.5-1mL of glycol solution, and then carrying out ultrasonic dissolution for 5-10min; adding starch solution, using a silver electrode as an indicating electrode and a calomel electrode as a reference electrode, adding sodium chloride standard solution with the same volume twice, and titrating with silver nitrate solution to an endpoint under the stirring condition to respectively obtain the volume of consumed silver nitrate solution at the endpoint of the twice titration; the volume of consumed silver nitrate solution and the concentration of the silver nitrate solution at the end point of the two titrations are obtained through blank test titration; calculating to obtain the content of chloride ions in the additive; the method has the problem that sediment adheres to the electrode during titration, thereby causing interference to measurement.
Therefore, developing a method for ensuring that chloride ions in cyclobenzaprine hydrochloride can be rapidly and effectively measured is an important point of research in the field of pharmaceutical analysis.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for detecting the content of chloride ions in cyclobenzaprine hydrochloride. The detection method has the characteristics of high accuracy, quick analysis, strong anti-interference performance and high sensitivity.
To achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a method for detecting the chloride ion content in cyclobenzaprine hydrochloride. The method for detecting the chloride ion content in cyclobenzaprine hydrochloride comprises the following steps:
(1) Sample preparation: mixing cyclobenzaprine hydrochloride, nitric acid, a nonionic surfactant and water to obtain a sample solution;
(2) Potentiometric titration analysis: and titrating the sample solution by adopting silver nitrate solution, and calculating to obtain the chloride ion content.
According to the invention, by adding the nonionic surfactant, the dissolution of the sample can be accelerated, the interference of the adhesion of the precipitate on the electrode in the titration process on the measurement is greatly eliminated, and the quick and effective measurement of chloride ions in cyclobenzaprine hydrochloride is ensured. Therefore, the detection method provided by the invention has the characteristics of high accuracy, rapid analysis, strong anti-interference performance and high sensitivity.
Wherein, the volume V of silver nitrate consumed by titration needs to be recorded AgNO3 The method comprises the steps of carrying out a first treatment on the surface of the And calculating the mass of chloride ions in the sample solution according to the following formula:
W Cl - ＝C AgNO3 ×V AgNO3 ×35.45；
wherein C is AgNO3 Representing the concentration (mol/L) of silver nitrate, V AgNO3 Represents the volume of silver nitrate (mL) consumed by titration, W Cl - Representing the mass (mg) of chloride ions in the sample solution.
The percentage content (% w/w Cl) of chloride ions in cyclobenzaprine hydrochloride is obtained by the following conversion - )：
％w/w Cl - ＝W Cl - ×100/W Sample of ；
Wherein W is Sample of Represents the mass (mg) of ciprofloxacin hydrochloride in the sample solution.
Preferably, in the step (1), the sample solution comprises the following components in percentage by mass: 0.05 to 0.3 percent of cyclobenzaprine hydrochloride, 0.5 to 3 percent of nitric acid, 0.05 to 5 percent of nonionic surfactant and 90 to 99 percent of water.
The content of cyclobenzaprine hydrochloride is 0.05-0.3%, for example, 0.05%, 0.1%, 0.15%, 0.2%, 0.25%, 0.3%, etc., based on 100% of the sample solution.
The content of the nitric acid is 0.5 to 3%, for example, 0.5%, 0.6%, 0.8%, 1%, 1.5%, 2%, 2.5%, 3%, etc., based on 100% by mass of the sample solution.
The nonionic surfactant may be contained in an amount of 0.05 to 5%, for example, 0.05%, 0.1%, 0.5%, 1%, 2%, 3%, 4%, 5%, etc., based on 100% by mass of the sample solution.
The water content is 90 to 99% by mass of the sample solution to be tested, and may be, for example, 90%, 91%, 92%, 93%, 94%, 95%, 96%, 97%, 98%, 99% by mass, or the like.
Preferably, in the step (1), the nonionic surfactant comprises any one or a combination of at least two of triton X-100, polyethylene glycol or polyvinylpyrrolidone, preferably triton X-100.
Preferably, in the step (1), the concentration of the nitric acid is 14.4-15.2mol/L, for example, 14.4mol/L, 14.5mol/L, 14.6mol/L, 14.7mol/L, 14.8mol/L, 14.9mol/L, 15.0mol/L, 15.1mol/L, 15.2mol/L and the like.
The concentration of nitric acid is defined herein as the concentration of nitric acid used, i.e., the concentration of nitric acid itself added at 0.5-3%, and not the concentration thereof in the sample solution, i.e., the concentration of pure HNO of the present invention at 0.5-3% at 14.4-15.2mol/L in the sample solution, because nitric acid is a distinction between concentrated nitric acid and dilute nitric acid 3 。
Preferably, in the step (1), the specific steps of preparing the sample for test are: firstly, mixing cyclobenzaprine hydrochloride with water, then adding nitric acid and a nonionic surfactant, and stirring to obtain the sample solution.
Preferably, in the step (2), the concentration of the silver nitrate solution is 0.05 to 0.2mol/L, for example, 0.05mol/L, 0.06mol/L, 0.08mol/L, 0.1mol/L, 0.12mol/L, 0.14mol/L, 0.16mol/L, 0.18mol/L, 0.2mol/L, etc., preferably 0.1mol/L.
Preferably, in the step (2), the electrode used in the titration is a composite silver-plated platinum ring electrode.
Preferably, the model of the composite silver-plated platinum ring electrode is DMi141-SC.
Preferably, in step (2), the titration is performed using a mertler potentiometric titrator T50.
Preferably, in step (2), the titrated reference electrolyte is a potassium nitrate solution.
Preferably, the concentration of the potassium nitrate solution is 0.5 to 2mol/L, for example, 0.5mol/L, 0.6mol/L, 0.8mol/L, 1mol/L, 1.2mol/L, 1.4mol/L, 1.6mol/L, 1.8mol/L, 2mol/L, etc., preferably 1mol/L.
Preferably, the titration is performed with stirring at a rotational speed of 20-50%, for example 20%, 25%, 30%, 35%, 40%, 45%, 50% etc.
Preferably, in step (2), the endpoint recognition threshold of the titration is 80-150mV/mL, which may be, for example, 80mV/mL, 85mV/mL, 90mV/mL, 95mV/mL, 100mV/mL, 110mV/mL, 120mV/mL, 130mV/mL, 140mV/mL, 150mV/mL, etc., preferably 100mV/mL.
Preferably, the method for detecting the chloride ion content in cyclobenzaprine hydrochloride comprises the following steps:
(1) Sample preparation: firstly, mixing cyclobenzaprine hydrochloride with water, then adding nitric acid and a nonionic surfactant, and stirring to obtain a sample solution;
wherein, the sample solution comprises the following components in percentage by mass: 0.05-0.3% of cyclobenzaprine hydrochloride, 1-3% of nitric acid, 0.05-5% of nonionic surfactant and 90-99% of water;
(2) Potentiometric titration analysis: titrating the sample solution by adopting 0.05-0.2mol/L silver nitrate solution, and calculating to obtain the chloride ion content;
wherein the electrode is a composite silver ring intelligent electrode DMi141-SC, the reference electrolyte is a potassium nitrate solution with the concentration of 0.5-2mol/L, the stirring speed is 20-50%, and the end point identification threshold value is 50-150mV/mL.
In addition, in the invention, a mode of titrating a sodium chloride standard solution by adopting a silver nitrate solution is adopted to examine the repeatability, the specificity, the linearity, the recovery rate and the like of a test method, and the specific titration method is the same as the detection method of the chloride ion content in the cyclobenzaprine hydrochloride.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the nonionic surfactant is added, so that the dissolution of a sample can be accelerated, the interference of the adhesion of the precipitate on the electrode in the titration process on the measurement is greatly eliminated, and the quick and effective measurement of chloride ions in cyclobenzaprine hydrochloride is ensured.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
The test instruments used in the following examples are as follows:
potentiometric titrator: a mertler potentiometric titrator T50; an electrode: composite silver ring intelligent electrode DMi141-SC; electromagnetic stirrer: a stirrer covered with polyethylene.
The sources of the components used in the following examples are as follows:
cyclobenzaprine hydrochloride (manufacturer: medichem, batch number: A-190305)&A-190306); triton X-100 (manufacturer: SIGMA-ALDRICH, viscosity: 243-291 cps); polyethylene glycol 400 (manufacturer: DOW, molecular weight: 396); polyvinylpyrrolidone (manufacturer: JRS, molecular weight: 3.8X10) 4 ) The method comprises the steps of carrying out a first treatment on the surface of the Nitric acid (manufacturer: national medicine group chemical reagent Co., ltd., concentration: 65.0-68.0 wt%); silver nitrate (manufacturer: shanghai city metering test technical institute, concentration: 0.1006 mol/L).
Example 1
The embodiment provides a method for detecting the content of chloride ions in cyclobenzaprine hydrochloride, which specifically comprises the following steps:
(1) Sample preparation: transferring about 200mg cyclobenzaprine hydrochloride batch 1 to a suitable beaker, adding 200mL of water to the beaker, stirring with a stirring magnet until dissolved, adding 5mL of nitric acid and 4mL of triton X-100 solution (5 wt%) to obtain the sample solution;
(2) Potentiometric titration analysis: titrating the sample solution by adopting 0.1mol/L silver nitrate solution, and calculating to obtain the chloride ion content;
wherein the electrode is a composite silver ring intelligent electrode DMi141-SC, the reference electrolyte is 1mol/L potassium nitrate solution, the stirring speed is 30%, and the end point identification threshold is 100mV/mL.
Example 2
The embodiment provides a method for detecting the content of chloride ions in cyclobenzaprine hydrochloride, which specifically comprises the following steps:
(1) Sample preparation: transferring about 200mg cyclobenzaprine hydrochloride batch 2 to a suitable beaker, adding 200mL of water to the beaker, stirring with a stirring magnet until dissolved, adding 6mL of nitric acid and 3mL of triton X-100 solution (5 wt%) to obtain the sample solution;
(2) Potentiometric titration analysis: titrating the sample solution by adopting 0.1mol/L silver nitrate solution, and calculating to obtain the chloride ion content;
wherein the electrode is a composite silver ring intelligent electrode DMi141-SC, the reference electrolyte is 1mol/L potassium nitrate solution, the stirring speed is 40%, and the end point identification threshold is 100mV/mL.
Example 3
The embodiment provides a method for detecting the content of chloride ions in cyclobenzaprine hydrochloride, which specifically comprises the following steps:
(1) Sample preparation: transferring about 200mg cyclobenzaprine hydrochloride batch 1 into a suitable beaker, adding 200mL of water into the beaker, stirring with a stirring magnet until the water is dissolved, and adding 5mL of nitric acid and 4mL of polyethylene glycol to obtain the sample solution;
(2) Potentiometric titration analysis: titrating the sample solution by adopting 0.1mol/L silver nitrate solution, and calculating to obtain the chloride ion content;
wherein the electrode is a composite silver ring intelligent electrode DMi141-SC, the reference electrolyte is 1mol/L potassium nitrate solution, the stirring speed is 40%, and the end point identification threshold is 100mV/mL.
Example 4
The embodiment provides a method for detecting the content of chloride ions in cyclobenzaprine hydrochloride, which specifically comprises the following steps:
(1) Sample preparation: transferring about 200mg cyclobenzaprine hydrochloride batch 1 to a suitable beaker, adding 200mL of water to the beaker, stirring with a stirring magnet until dissolved, and adding 5mL of nitric acid and 4mL of polyvinylpyrrolidone solution (5 wt%) to obtain the sample solution;
(2) Potentiometric titration analysis: titrating the sample solution by adopting 0.1mol/L silver nitrate solution, and calculating to obtain the chloride ion content;
wherein the electrode is a composite silver ring intelligent electrode DMi141-SC, the reference electrolyte is 1mol/L potassium nitrate solution, the stirring speed is 40%, and the end point identification threshold is 100mV/mL.
Example 5
The embodiment provides a method for detecting the content of chloride ions in cyclobenzaprine hydrochloride, which specifically comprises the following steps:
(1) Sample preparation: transferring about 200mg cyclobenzaprine hydrochloride batch 1 to a suitable beaker, adding 200mL of water to the beaker, stirring with a stirring magnet until dissolved, adding 5mL of nitric acid and 1mL of triton X-100 solution (5 wt%) to obtain the sample solution;
(2) Potentiometric titration analysis: titrating the sample solution by adopting 0.1mol/L silver nitrate solution, and calculating to obtain the chloride ion content;
wherein the electrode is a composite silver ring intelligent electrode DMi141-SC, the reference electrolyte is 1mol/L potassium nitrate solution, the stirring speed is 30%, and the end point identification threshold is 100mV/mL.
Example 6
The embodiment provides a method for detecting the content of chloride ions in cyclobenzaprine hydrochloride, which specifically comprises the following steps:
(1) Sample preparation: transferring about 200mg cyclobenzaprine hydrochloride batch 1 to a suitable beaker, adding 200mL of water to the beaker, stirring with a stirring magnet until dissolved, adding 5mL of nitric acid and 10mL of triton X-100 solution (5 wt%) to obtain the sample solution;
(2) Potentiometric titration analysis: titrating the sample solution by adopting 0.1mol/L silver nitrate solution, and calculating to obtain the chloride ion content;
wherein the electrode is a composite silver ring intelligent electrode DMi141-SC, the reference electrolyte is 1mol/L potassium nitrate solution, the stirring speed is 30%, and the end point identification threshold is 100mV/mL.
Example 7
The embodiment provides a method for detecting the content of chloride ions in cyclobenzaprine hydrochloride, which specifically comprises the following steps:
(1) Sample preparation: transferring about 200mg cyclobenzaprine hydrochloride batch 1 to a suitable beaker, adding 200mL of water to the beaker, stirring with a stirring magnet until dissolved, adding 5mL of nitric acid and 4mL of triton X-100 solution (5 wt%) to obtain the sample solution;
(2) Potentiometric titration analysis: titrating the sample solution by adopting 0.1mol/L silver nitrate solution, and calculating to obtain the chloride ion content;
the silver electrode is used as an indicating electrode, the double-salt bridge type saturated calomel electrode is used as a reference electrode, 3mol/L potassium chloride solution is added into a first salt bridge of the double-salt bridge type saturated calomel electrode, 0.1mol/L potassium nitrate solution is added into a second salt bridge, the stirring rotating speed is 30%, and the end point identification threshold value is 100mV/mL.
Comparative example 1
The comparative example provides a method for detecting the content of chloride ions in cyclobenzaprine hydrochloride, which specifically comprises the following steps:
(1) Sample preparation: transferring about 200mg cyclobenzaprine hydrochloride batch 1 into a proper beaker, adding 200mL of water into the beaker, stirring with a stirring magnet until the water is dissolved, and adding 5mL of nitric acid to obtain the sample solution;
(2) Potentiometric titration analysis: titrating the sample solution by adopting 0.1mol/L silver nitrate solution;
wherein the electrode is a composite silver ring intelligent electrode DMi141-SC, the reference electrolyte is 1mol/L potassium nitrate solution, the stirring speed is 30%, and the end point identification threshold is 100mV/mL. The method comprises the steps of carrying out a first treatment on the surface of the
The result shows that: the titration endpoint cannot be reached.
Comparative example 2
The comparative example provides a method for detecting the content of chloride ions in cyclobenzaprine hydrochloride, which specifically comprises the following steps:
(1) Sample preparation: transferring about 200mg cyclobenzaprine hydrochloride batch 1 to a suitable beaker, adding 200mL of water to the beaker, stirring with a stirring magnet until dissolved, adding 5mL of nitric acid and 4mL of sodium dodecylbenzenesulfonate (5 wt%) to obtain the sample solution;
(2) Potentiometric titration analysis: titrating the sample solution by adopting 0.1mol/L silver nitrate solution;
wherein the electrode is a composite silver ring intelligent electrode DMi141-SC, the reference electrolyte is 1mol/L potassium nitrate solution, the stirring speed is 30%, and the end point identification threshold is 100mV/mL.
The result shows that: the titration endpoint cannot be reached.
Comparative example 3
The comparative example provides a method for detecting the content of chloride ions in cyclobenzaprine hydrochloride, which specifically comprises the following steps:
(1) Preparation of the microemulsion: the optimal proportion of the preparation table is deionized water, triton X-100, cyclohexane, and surface active mixed liquid of n-butanol=3:4:4:2 (volume ratio);
(2) Preparation of silver nitrate solution: accurately weighing 169.87mg of dried silver nitrate solid, fully dissolving the silver nitrate solid with deionized water, then fixing the solution in a volumetric flask of 100mL to prepare a standard 0.01mol/L silver nitrate reagent, and placing the silver nitrate reagent in a brown bottle and placing the brown bottle in a light-proof place;
(3) Preparation of nitric acid diluent: 50mL of analytically pure nitric acid is taken and added with 50mL of water to obtain a diluent, wherein the mass fraction of the analytically pure nitric acid is 65%.
(4) Preparing a stable silver chloride suspension: absorbing a certain volume of chloride ion standard solution in a brown colorimetric tube, adding 2mL of the nitric acid solution prepared in the step (3), 2mL of the microemulsion prepared in the step (1) and 2mL of the silver nitrate solution prepared in the step (2) into the colorimetric tube, adding deionized water to a calibrated scale mark, shaking uniformly, placing the materials in a light-shielding place for standing for 15min, absorbing a proper amount of silver chloride suspension generated by reaction by using a disposable plastic dropper, and transferring the silver chloride suspension into a colorimetric tube with the thickness of 10 mm;
(5) Determination of detection wavelength
And (3) preparing a proper amount of 1mg/L chloride ion standard solution into a stable silver chloride suspension according to the step (4), and collecting a spectrum absorption curve of the suspension within a range of 360-900 nm through a spectrometer.
(6) Drawing a standard curve chart of chloride ion content and absorbance: taking 7 25mL brown color comparison tubes, respectively attaching labels of 0mg/L, 1mg/L and 2mg/L … … mg/L on the brown color comparison tubes, sequentially adding standard chloride ion solutions with volumes of 0, 1, 2, 3, 4, 5 and 6mL, sequentially adding 4mL of the dilute solution prepared in the step (3), 2mL of the microemulsion prepared in the step (1) and 2mL of the silver nitrate solution prepared in the step (2) according to an experimental method, using deionized water to fix the volume to the scale mark of the brown color comparison tubes, shaking uniformly, placing the mixture in a dark place for 15min, collecting absorbance of the reacted solution in each color comparison tube at 420nm through a spectrometer, and establishing a quantitative model between the chloride ion content and the absorbance;
(7) Preparation and testing of sample solutions: accurately weighing 4mg of ciprofloxacin hydrochloride, fully dissolving with deionized water, then fixing the solution in a 200mL volumetric flask, and sequentially adding 4mL of the nitric acid diluent prepared in the step (3), 2mL of the microemulsion prepared in the step (1) and 2mL of the silver nitrate solution prepared in the step (2) according to an experimental method.
The result shows that: the solution for the sample cannot form stable suspension, the absorbance is reduced along with the time, and the content of chloride ions cannot be measured by spectrophotometry.
Methodology investigation
The method for detecting the chloride ion content in cyclobenzaprine hydrochloride provided in the above examples 1 to 7 was examined in methodology, and the specific test method is as follows:
(1) Preparing a reference substance solution: accurately weighing 770mg of sodium chloride into 200mL measuring flask, and dissolving with water to constant volume to scale. The solution is a reference stock solution. Measuring the reference stock solution in a measuring flask with 10mL to 200mL, diluting with water to a scale, and shaking uniformly. The solution in the measuring flask is completely transferred to a proper beaker, 3-8mL of nitric acid and 2-6mL of triton X-100 solution (5%) are added and stirred uniformly to be used as a reference solution for analysis.
(2) The testing method comprises the following steps:
sample introduction reproducibility: continuously analyzing 3 parts of the reference substance solution, and calculating the recovery rate of chloride ions in the sodium chloride solution;
specialization: testing whether the blank solution (except for the cyclobenzaprine hydrochloride, the concentrations of the other components and the components are completely consistent with those of the sample in the corresponding examples 1-7) has response to chloride ions; wherein, NO represents NO obvious response of chloride ions in the blank solution, YES represents obvious response of chloride ions in the blank solution;
linearity: seven chloride ion masses (examples 1:9.976-29.929mg; examples 2:9.594-28.782mg; examples 3:10.091-30.272mg; examples 4:9.646-28.938mg; examples 5:10.118-30.354mg; examples 6:9.516-28.548mg; examples 7:9.755-29.265 mg) were examined, and each consumption was fitted to the corresponding chloride ion mass with a linear equation;
recovery rate: recovery at three concentration levels (50 mg/mL, 100mg/mL, 150 mg/mL) was examined;
repeatability: preparing 6 parts of sample solutions for sample solutions adopted in corresponding examples in parallel, and calculating RSD of a chloride ion measurement result;
intermediate precision: preparing six samples in parallel on different days by a second tester, and calculating RSD of a chloride ion measurement result;
durability: samples were prepared in triplicate at 150mg and 250mg, respectively, for the difference between chloride ion assay and reproducibility.
The specific test results are shown in table 1 below:
TABLE 1
As can be seen from the test data in table 1, sample injection reproducibility: 3 parts of control solution are continuously analyzed, and the recovery rate of chloride ions in the sodium chloride solution is calculated, wherein the recovery rate is between 95.0% and 105.0%, and the% RSD is less than 2.5, which proves that the repeatability of the detection method is excellent.
Specialization: the blank solutions (except for the cyclobenzaprine hydrochloride, the concentrations of the other components and the components are completely consistent with those of the sample in the corresponding examples 1-7) are analyzed and tested, and the blank solvents adopted in the examples have no chloride ion response, so that the specificity of the detection method disclosed by the invention is excellent.
Linearity: the consumption of the silver nitrate solution at seven concentration levels is examined, and the correlation coefficient of the results is above 0.999, which shows that the detection method has excellent linearity.
Recovery rate: recovery at three concentration levels (50-150 mg/mL) was examined, with results ranging from 95.0% to 105.0% and% RSD less than 2.5.
Repeatability: 6 samples were prepared in parallel and the% RSD of the chloride ion assay was less than 3.0.
Intermediate precision: six samples were prepared in parallel on different days by a second tester, with a% RSD of less than 5.0 for the chloride ion assay and no more than 0.3% difference in chloride ion content compared to the repeat results.
Durability: three samples, 150mg and 250mg, were prepared in parallel, and the chloride ion assay results were not more than 0.3% different from the reproducibility results.
In summary, in the invention, by adding the nonionic surfactant, the dissolution of the sample can be accelerated, the interference of the sediment adhered to the electrode in the titration process on the measurement is greatly eliminated, and the quick and effective measurement of chloride ions in cyclobenzaprine hydrochloride is ensured. Therefore, the detection method provided by the invention has the characteristics of high accuracy, rapid analysis, strong anti-interference performance and high sensitivity.
The applicant states that the method for detecting the chloride ion content in cyclobenzaprine hydrochloride according to the present invention is described by the above examples, but the present invention is not limited to the above examples, i.e. it does not mean that the present invention must be carried out by depending on the above examples. It should be apparent to those skilled in the art that any modification of the present invention, equivalent substitution of raw materials for the product of the present invention, addition of auxiliary components, selection of specific modes, etc., falls within the scope of the present invention and the scope of disclosure.
Claims (15)
1. The method for detecting the content of chloride ions in cyclobenzaprine hydrochloride is characterized by comprising the following steps of:
(1) Sample preparation: mixing cyclobenzaprine hydrochloride, nitric acid, a nonionic surfactant and water to obtain a sample solution; the sample solution comprises the following components in percentage by mass: 0.05-0.3% of cyclobenzaprine hydrochloride, 0.5-3% of nitric acid, 0.05-5% of nonionic surfactant and 90-99% of water; the nonionic surfactant comprises any one or a combination of at least two of triton X-100, polyethylene glycol or polyvinylpyrrolidone;
(2) Potentiometric titration analysis: and titrating the sample solution by adopting silver nitrate solution, and calculating to obtain the chloride ion content.
2. The method for detecting chloride ion content in cyclobenzaprine hydrochloride according to claim 1, wherein in the step (1), the nonionic surfactant is triamcinolone acetonide X-100.
3. The method for detecting chloride ion content in cyclobenzaprine hydrochloride according to claim 1, wherein in the step (1), the concentration of the nitric acid is 14.4-15.2mol/L.
4. The method for detecting chloride ion content in cyclobenzaprine hydrochloride according to claim 1, wherein in the step (1), the specific steps for preparing the sample are as follows: firstly, mixing cyclobenzaprine hydrochloride with water, then adding nitric acid and a nonionic surfactant, and stirring to obtain the sample solution.
5. The method for detecting chloride ion content in cyclobenzaprine hydrochloride according to claim 1, wherein in the step (2), the concentration of the silver nitrate solution is 0.05-0.2mol/L.
6. The method for detecting chloride ion content in cyclobenzaprine hydrochloride according to claim 1, wherein in the step (2), the concentration of the silver nitrate solution is 0.1mol/L.
7. The method for detecting chloride ion content in cyclobenzaprine hydrochloride according to claim 1, wherein in the step (2), the electrode used for titration is a composite silver-plated platinum ring electrode.
8. The method for detecting the chloride ion content in cyclobenzaprine hydrochloride according to claim 7, wherein the composite silver-plated platinum ring electrode is of the model number DMi141-SC.
9. The method for detecting chloride ion content in cyclobenzaprine hydrochloride according to claim 1, wherein in the step (2), the titration is performed by a mertler potentiometric titrator T50.
10. The method for detecting chloride ion content in cyclobenzaprine hydrochloride according to claim 1, wherein in the step (2), the titrated reference electrolyte is a potassium nitrate solution.
11. The method for detecting chloride ion content in cyclobenzaprine hydrochloride according to claim 10, wherein the concentration of the potassium nitrate solution is 0.5-2mol/L.
12. The method for detecting chloride ion content in cyclobenzaprine hydrochloride according to claim 10, wherein the concentration of the potassium nitrate solution is 1mol/L.
13. The method for detecting chloride ion content in cyclobenzaprine hydrochloride according to claim 1, wherein in the step (2), the endpoint recognition threshold of the titration is 80-150mV/mL.
14. The method for detecting chloride ion content in cyclobenzaprine hydrochloride according to claim 1, wherein in the step (2), the endpoint recognition threshold of the titration is 100mV/mL.
15. The method for detecting the content of chloride ions in cyclobenzaprine hydrochloride according to claim 1, wherein the method for detecting the content of chloride ions in cyclobenzaprine hydrochloride comprises the following steps:
(1) Sample preparation: firstly, mixing cyclobenzaprine hydrochloride with water, then adding nitric acid and a nonionic surfactant, and stirring to obtain a sample solution;
wherein, the sample solution comprises the following components in percentage by mass: 0.05-0.3% of cyclobenzaprine hydrochloride, 1-3% of nitric acid, 0.05-5% of nonionic surfactant and 90-99% of water;
(2) Potentiometric titration analysis: titrating the sample solution by adopting 0.05-0.2mol/L silver nitrate solution, and calculating to obtain the chloride ion content;
wherein, the titration adopts a Metler potential titration instrument T50, the electrode is a composite silver ring intelligent electrode DMi141-SC, the reference electrolyte is a potassium nitrate solution with the concentration of 0.5-2mol/L, the stirring speed is 20-50%, and the end point identification threshold value is 50-150mV/mL.
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