Method for testing impurity content in trifluoroethylamine hydrochloride

Abstract

The invention discloses a method for testing the content of impurities in trifluoroethylamine hydrochloride. The method comprises the following steps: (1) preparing a sodium hydroxide solution as a diluent; (2) respectively dissolving a trifluoroethylamine hydrochloride test sample and a reference substance in a diluent to obtain a test sample solution and a reference substance solution; and (3) carrying out sample injection detection on the test solution and the reference solution by adopting a headspace gas chromatography, and calculating the impurity content in the trifluoroethylamine hydrochloride according to a main component external standard method. According to the method, trifluoroethylamine in the trifluoroethylamine hydrochloride is dissociated by using the sodium hydroxide solution, and then is detected by adopting the gas chromatography, so that the problems of relatively poor peak shape and baseline are solved, and the method is simple and convenient to operate and relatively high in universality, and can be used for quality control and evaluation of the trifluoroethylamine hydrochloride.

Description

Technical Field

[0001] The present invention relates to the technical field of pharmaceutical analysis, and particularly to a method for testing the impurity content in trifluoroethylamine hydrochloride. Background Art

[0002] Trifluoroethylamine hydrochloride has the molecular formula C 2 H 5 ClF 3 N, with a molecular weight of 135.52, and its chemical structural formula is as follows:

[0003] In the existing art of the synthesis method of upadacitinib, trifluoroethylamine hydrochloride is generally used as an important starting material for the synthesis of upadacitinib, such as the synthesis methods of upadacitinib disclosed in patents CN111217819B and CN117285537B. Therefore, the purity of trifluoroethylamine hydrochloride directly affects the product quality of upadacitinib. Currently, the existing technologies mainly focus on the synthesis of trifluoroethylamine, and there is relatively little research on the detection methods for related impurities in trifluoroethylamine hydrochloride.

[0004] Trifluoroethylamine hydrochloride has no ultraviolet absorption, so the conventional liquid chromatography method with UV detector cannot be used; when directly injecting samples by gas chromatography, due to the relatively high boiling point of trifluoroethylamine hydrochloride, the peak shape is poor, and it is impossible to accurately quantify the impurities. Moreover, the salt is easily retained in the liner and chromatographic column, affecting the service life.

[0005] Therefore, in order to control the quality of drugs and improve drug safety, it is necessary to develop a simple and accurate method for detecting related substances in trifluoroethylamine hydrochloride. Summary of the Invention

[0006] The present invention aims to overcome the problem of the method for related impurities in trifluoroethylamine hydrochloride that cannot be accurately determined in the prior art, and provides a method for testing the impurity content in trifluoroethylamine hydrochloride. After trifluoroethylamine hydrochloride is freed by sodium hydroxide solution, gas chromatography is used for detection, solving the problems of poor peak shape and baseline. The method of the present invention is simple to operate and has strong generality, and can be used for the quality control and evaluation of trifluoroethylamine hydrochloride.

[0007] In order to achieve the above object, the present invention adopts the following technical solutions: A method for testing the impurity content in trifluoroethylamine hydrochloride, comprising the following steps: (1) Prepare a sodium hydroxide solution as a diluent; (2) Dissolve the test sample and reference substance of trifluoroethylamine hydrochloride in the diluent respectively to obtain a test sample solution and a reference substance solution; (3) The headspace gas chromatography method is used to inject and detect the test solution and the reference solution, and the impurity content in trifluoroethylamine hydrochloride is calculated according to the external standard method of the main component.

[0008] In the present invention, a sodium hydroxide solution is used as a diluent. After the trifluoroethylamine in trifluoroethylamine hydrochloride is liberated with the sodium hydroxide solution, gas chromatography is used for detection, which can solve the problems of poor peak shape and baseline, and has good specificity, accuracy, detection limit and quantification limit; the system suitability meets the requirements. The method of the present invention is simple to operate and has strong generality, and can be used for the quality control and evaluation of trifluoroethylamine hydrochloride.

[0009] Preferably, in step (1), the concentration of the sodium hydroxide solution is 0.09 - 0.11 g / mL.

[0010] Preferably, in the test solution in step (2), the concentration of the trifluoroethylamine hydrochloride test sample is 95 - 105 mg / mL.

[0011] Preferably, in the reference solution in step (2), the concentration of the trifluoroethylamine hydrochloride reference is 0.08 - 0.12 mg / mL.

[0012] Preferably, the gas chromatography conditions in step (3) include: the initial temperature is 40 ± 2 °C, maintained for 4 - 6 minutes, heated at a rate of 5 ± 1 °C per minute to 55 - 65 °C, and then heated at a rate of 40 ± 5 °C per minute to 240 - 245 °C, maintained for 4 - 6 minutes.

[0013] Preferably, the gas chromatography conditions in step (3) include: the column flow rate is 2 - 4 mL / min, the split ratio is 18 - 22:1; a capillary column with 4 - 6 wt% cyanopropylphenyl and 94 - 96 wt% polydimethylsiloxane as the stationary liquid is used; the inlet temperature is 195 - 205 °C, and the carrier gas is nitrogen.

[0014] Preferably, the capillary column is DB-624, with a length of 30 m, an inner diameter of 0.53 mm, and a film thickness of 3.0 μm.

[0015] Preferably, the headspace conditions for gas chromatography in step (3) include: the sample equilibrium temperature is 80 ± 2 °C; the transfer line temperature is 100 ± 2 °C; the quantitative loop temperature is 90 ± 2 °C; the headspace equilibrium time is 28 - 32 minutes; the cycle time is 20 - 30 minutes.

[0016] Preferably, the calculation formula for the impurity content in step (3) is: Wherein, As: the peak area of each impurity in the test solution; A R : the peak area of the main component in the reference solution; W R : The weighed amount of the reference substance, mg; W S : The weighed amount of the test sample, mg; D R : The dilution factor of the reference substance solution; D S : The dilution factor of the sample; P: The content of the main component in the reference substance.

[0017] Therefore, the present invention has the following beneficial effects: The method of the present invention has good specificity, accuracy, detection limit and quantitation limit, and the system suitability meets the requirements; and it is easy to operate, has strong generality, and can be used for the quality control and evaluation of trifluoroethylamine hydrochloride. Description of the Drawings

[0018] Figure 1 It is the gas chromatogram of the blank solution in Example 1.

[0019] Figure 2 It is the gas chromatogram of the system suitability solution in Example 1.

[0020] Figure 3 It is the gas chromatogram of the test sample solution in Example 1.

[0021] Figure 4 It is the gas chromatogram of the system suitability solution in Comparative Example 1. Detailed Embodiments

[0022] The present invention will be further described below in conjunction with the drawings and specific embodiments.

[0023] In the present invention, unless otherwise specified, all equipment and raw materials can be purchased from the market or are commonly used in this industry. The methods in the following examples, unless otherwise specified, are conventional methods in this field.

[0024] In order to further understand the present invention, the preferred embodiments of the present invention will be described below in conjunction with specific embodiments. However, it should be understood that these descriptions are only for further explaining the features and advantages of the present invention rather than limiting the claims of the present invention.

[0025] Many specific details are set forth in the following description in order to fully understand the present invention. However, the present invention can also be implemented in other ways different from those described herein. Those skilled in the art can make similar generalizations without departing from the connotation of the present invention. Therefore, the present invention is not limited by the specific embodiments disclosed below.

[0026] Second, the "one embodiment" or "embodiment" mentioned herein refers to specific features, structures, or characteristics that may be included in at least one implementation manner of the present invention. The "in one embodiment" that appears in different places in this specification does not all refer to the same embodiment, nor is it a separate or alternative embodiment that is mutually exclusive with other embodiments.

[0027] In the embodiments of the present invention, the names and structural formulas of the related impurities of trifluoroethylamine hydrochloride are shown in Table 1; the experimental instruments, as well as the information of the test drugs and reagents used, are shown in Tables 2 and 3 respectively.

[0028] Table 1: Related impurities of trifluoroethylamine hydrochloride.

[0029] Table 2: Experimental instruments. Instrument Model Manufacturer Whether it meets the verification standard Electronic balance XPR205 / A Mettler Yes Gas chromatograph 7890B Agilent Yes

[0030] Table 3: Test drugs and reagents. Reagent name Batch number Purity Manufacturer Sodium hydroxide 20230406 Analytical reagent Sinopharm Group Trifluoroethylamine 24U2121-0423A2 100％ TP Standards GmaH Trifluoroethanol O13URXAR Analytical reagent Anychem

[0031] General embodiment: A method for testing the impurity content in trifluoroethylamine hydrochloride, comprising the following steps: (1) Prepare a sodium hydroxide solution as a diluent; (2) Dissolve the trifluoroethylamine hydrochloride test sample and the reference substance in the diluent respectively to obtain a test sample solution and a reference substance solution; (3) Use headspace gas chromatography to inject and detect the test sample solution and the reference substance solution, and calculate the impurity content in trifluoroethylamine hydrochloride according to the external standard method for the main component.

[0032] As a specific implementation manner, in step (1), the concentration of the sodium hydroxide solution is 0.09 - 0.11 g / mL.

[0033] As a specific implementation manner, in the test sample solution in step (2), the concentration of the trifluoroethylamine hydrochloride test sample is 95 - 105 mg / mL.

[0034] As a specific implementation manner, in the reference substance solution in step (2), the concentration of the trifluoroethylamine hydrochloride reference substance is 0.08 - 0.12 mg / mL.

[0035] As a specific implementation manner, the gas chromatography conditions in step (3) include: an initial temperature of 40 ± 2 °C, maintained for 4 - 6 minutes, heated at a rate of 5 ± 1 °C per minute to 55 - 65 °C, and then heated at a rate of 40 ± 5 °C per minute to 240 - 245 °C, maintained for 4 - 6 minutes.

[0036] As a specific embodiment, the gas chromatography conditions in step (3) include: the column flow rate is 2 - 4 mL / min, the split ratio is 18 - 22:1; a capillary column with 4 - 6 wt% cyanopropylphenyl and 94 - 96 wt% polydimethylsiloxane as the stationary liquid is used; the inlet temperature is 195 - 205 °C, and the carrier gas is nitrogen.

[0037] As a specific embodiment, the capillary column is DB - 624, with a length of 30 m, an inner diameter of 0.53 mm, and a film thickness of 3.0 μm.

[0038] As a specific embodiment, the headspace conditions for gas chromatography in step (3) include: the sample equilibrium temperature is 80 ± 2 °C; the transfer line temperature is 100 ± 2 °C; the quantitative loop temperature is 90 ± 2 °C; the headspace equilibrium time is 28 - 32 minutes; the cycle time is 20 - 30 minutes.

[0039] As a specific embodiment, the calculation formula for the impurity content in step (3) is: Wherein, As: the peak area of each impurity in the test solution; A R : the peak area of the main component in the reference solution; W R : the weighed amount of the reference substance, mg; W S : the weighed amount of the test substance, mg; D R : the dilution factor of the reference solution; D S : the dilution factor of the sample; P: the content of the main component in the reference substance.

[0040] Example 1: A method for testing the impurity content in trifluoroethylamine hydrochloride includes the following steps: Step 1: Preparation of solutions: Preparation of the diluent: Take 100 g of sodium hydroxide, add 1 L of water to dissolve it, and obtain a 0.1 g / mL sodium hydroxide solution as the diluent.

[0041] Blank solution: The diluent.

[0042] Test solution: Take 100 mg of the trifluoroethylamine hydrochloride test substance, place it in a 20 mL headspace vial, accurately add 1 mL of the diluent, and seal it.

[0043] Reference solution: Take 10 mg of trifluoroethylamine hydrochloride reference substance, place it in a 100 mL volumetric flask, dissolve it with the diluent and dilute it to the mark, shake well to obtain a 0.1 mg / mL trifluoroethylamine hydrochloride solution; accurately measure 1 mL and place it in a 20 mL headspace vial, and seal it.

[0044] Step 2: Use gas chromatography to detect the above reference solution and test solution: The gas chromatography detection conditions include: an initial temperature of 40 °C, maintained for 5 minutes, heated at a rate of 5 °C per minute to 60 °C, and then heated at a rate of 40 °C per minute to 240 °C, maintained for 5 minutes; The gas chromatography conditions also include a column flow rate of 3 mL / min and a split ratio of 20:1; a capillary column with 6 wt% cyanopropylphenyl and 94 wt% polydimethylsiloxane as the stationary liquid; the capillary column is DB-624 (30 m × 0.53 mm, 3.0 μm); in the gas chromatography detection conditions, the injection port temperature is 200 °C and the carrier gas is nitrogen; The gas chromatography headspace conditions include: a sample equilibrium temperature of 80 °C; a transfer line temperature of 100 °C; a quantitative loop temperature of 90 °C; a headspace equilibrium time of 30 minutes; a cycle time of 25 minutes.

[0045] Step 3: Calculate the related substance content in trifluoroethylamine hydrochloride according to the external standard method for the main component: The calculation formula is Where, As: the peak area of each impurity in the test solution; A R : the peak area of the main component of the reference solution; W R : the weighed amount of the reference substance, mg; W S : the weighed amount of the test sample, mg; D R : the dilution factor of the reference solution; D S : the dilution factor of the sample; P: the content of the main component in the reference substance.

[0046] The specificity and system suitability test of the method described in the present invention: System suitability solution: Take trifluoroethylamine reference substance and impurity reference substance respectively, and prepare a solution containing 100 mg / mL of trifluoroethylamine and 0.1 mg / mL of impurity with the diluent as the system suitability solution.

[0047] Use the above gas chromatography to detect the blank solution and the system suitability solution. The typical chromatogram of the blank solution is as Figure 1 shown, fromFigure 1 It can be seen that the blank solution does not interfere with the detection of the test sample. The typical chromatogram of the system suitability solution is as Figure 2 shown, and from Figure 2 it can be seen that the resolution between the impurities and the main peak in the system suitability solution meets the requirements.

[0048] Quantitation limit and detection limit tests of the method described in the present invention: Quantitation limit solution: Take trifluoroethylamine reference substance and impurity reference substance, and prepare a solution containing both trifluoroethylamine and trifluoroethanol at 0.01 mg / mL with the diluent as the quantitation limit solution.

[0049] Detection limit solution: Take appropriate amounts of trifluoroethylamine reference substance and impurity reference substance, and prepare a solution containing both trifluoroethylamine and trifluoroethanol at 0.003 mg / mL with the diluent as the detection limit solution.

[0050] The quantitation limit solution and the detection limit solution were detected by the above gas chromatography method, and the quantitation limit and detection limit were calculated according to the signal-to-noise ratio. The results are shown in Table 4.

[0051] Table 4: Test results of quantitation limit and detection limit.

[0052] It can be seen from the results in Table 4 that the sensitivity of the related substance impurities meets the detection requirements.

[0053] Linearity test of the method described in the present invention: Series of linear reference substance solutions: Take trifluoroethylamine reference substance and impurity reference substance, and prepare solutions containing trifluoroethylamine and trifluoroethanol at concentrations of 0.01 mg / mL, 0.05 mg / mL, 0.1 mg / mL, 0.15 mg / mL, and 0.2 mg / mL respectively with the diluent as linear solutions 1 - 5; Inject samples separately, record the chromatograms, and perform linear regression with the peak area against the concentration; The results are shown in Table 5.

[0054] Table 5: Linear range of trifluoroethylamine and trifluoroethanol. Name Regression equation Correlation coefficient Concentration (mg / mL) Trifluoroethylamine y = 8.3356x - 2.7875 0.9995 0.01005～0.2010 Trifluoroethanol y = 5.4866x - 0.3266 0.9992 0.01088～0.2176

[0055] It can be seen from Table 5 that within the range of 0.01% - 0.2% of the concentration equivalent to the test sample solution for trifluoroethanol, the peak area has a good linear relationship with the concentration, and the correlation coefficient is greater than 0.99, indicating a good linear relationship.

[0056] Accuracy test of the method described in the present invention: Reference substance solution (low concentration): Take 1 mg of trifluoroethanol reference substance, place it in a 100 mL volumetric flask, dissolve it with the diluent and dilute to the mark, and shake well.

[0057] Reference solution (medium concentration): Take 10 mg of trifluoroethanol reference substance, place it in a 100 mL volumetric flask, dissolve it with the diluent and dilute to the mark, then shake well.

[0058] Reference solution (high concentration): Take 10 mg of trifluoroethanol reference substance, place it in a 50 mL volumetric flask, dissolve it with the diluent and dilute to the mark, then shake well.

[0059] Accuracy solution: Take 100 mg of the test substance of trifluoroethylamine hydrochloride, place it in a 20 mL headspace vial, accurately add 1 mL of reference solutions with different concentrations, seal it; prepare three replicates for each concentration level; inject samples respectively, and calculate the recovery rate and RSD. The results are shown in Table 6.

[0060] Table 6: Results of accuracy test.

[0061] As can be seen from Table 6, the recovery rate of trifluoroethanol is between 95.3% and 100.2%, and the RSD of the recovery rate is less than 10%. The accuracy of this method meets the requirements.

[0062] Precision test of the method described in the present invention: Reference solution: Take 10 mg of trifluoroethanol reference substance, place it in a 100 mL volumetric flask, dissolve it with the diluent and dilute to the mark, then shake well.

[0063] Test solution: Take 100 mg of the test substance of trifluoroethylamine hydrochloride, place it in a 20 mL headspace vial, accurately add 1 mL of the reference solution, seal it; prepare six replicates; inject samples respectively to test the repeatability. The typical chromatogram of the test solution is as Figure 3 shown, and the repeatability results are shown in Table 7.

[0064] Table 7: Results of repeatability test.

[0065] As can be seen from the results in Table 7, the repeatability of the method of the present invention meets the requirements.

[0066] Solution stability test of the method described in the present invention: Take the repeatability solution and place it at room temperature for 24 h, inject 1 sample at different times; the solution stability test results are shown in Table 8.

[0067] Table 8: Results of solution stability test.

[0068] As can be seen from the results in Table 8: When the test solution is placed at room temperature for 24 h, the RSD of the determination result of trifluoroethanol < 0.01%, and the test solution is stable when placed at room temperature for 24 h.

[0069] Based on the above tests, it can be seen that the system suitability, specificity, linearity, accuracy, precision, and solution stability of this method all meet the requirements.

[0070] Comparative Example 1 (without adding sodium hydroxide): A method for testing the impurity content in trifluoroethylamine hydrochloride includes the following steps: Step 1: Preparation of solutions: Diluent: water.

[0071] Blank solution: diluent.

[0072] Test solution: Take 100 mg of the trifluoroethylamine hydrochloride test sample, place it in a 20 mL headspace vial, accurately add 1 mL of the diluent, and seal.

[0073] Reference solution: Take 10 mg of the trifluoroethylamine hydrochloride reference substance, place it in a 100 mL volumetric flask, dissolve it with the diluent and dilute to the mark, shake well to obtain a 0.1 mg / mL trifluoroethylamine hydrochloride solution; accurately measure 1 mL and place it in a 20 mL headspace vial, and seal.

[0074] Step 2: Detect the above reference solution and test solution by gas chromatography: The gas chromatography detection conditions include: initial temperature 35 °C, maintained for 10 min, heated at a rate of 5 °C per minute to 60 °C, maintained for 5 min, heated at a rate of 20 °C per minute to 240 °C, and held for 10 min; The gas chromatography conditions also include a column flow rate of 3 mL / min and a split ratio of 20:1; a capillary column with 6 wt% cyanopropylphenyl and 94 wt% polydimethylsiloxane as the stationary liquid; the capillary column is DB-624 (30 m × 0.53 mm, 3.0 μm); in the gas chromatography detection conditions, the injection port temperature is 250 °C, and the carrier gas is nitrogen; The gas chromatography headspace conditions include: sample equilibrium temperature 80 °C; transfer line temperature 100 °C; quantitative loop temperature 90 °C; headspace equilibrium time 30 minutes; cycle time 25 minutes.

[0075] Step 3: Calculate the related substance content in trifluoroethylamine hydrochloride according to the external standard method for the main component: The calculation formula is where As: the peak area of each impurity in the test solution; A R : the peak area of the main component in the reference solution; W R : the weighed amount of the reference substance, mg; W S: Sampling amount of the test sample, mg; D R : Dilution factor of the reference solution; D S : Dilution factor of the sample; P: Content of the main component in the reference substance.

[0076] System suitability test for the method described in Comparative Example 1: System suitability solution: Take trifluoroethylamine reference substance and impurity reference substance respectively, and prepare a solution containing 100 mg / mL of trifluoroethylamine and 0.1 mg / mL of impurity with the diluent as the system suitability solution.

[0077] Detect the system suitability solution by the above gas chromatography method. The typical chromatogram of the system suitability solution is as Figure 4 shown. It can be seen from Figure 4 that when sodium hydroxide is not added to the diluent in Comparative Example 1, the response of the main peak is low, and the peak shape and baseline are poor, not meeting the test requirements.

[0078] Quantitation limit and detection limit tests for the method described in Comparative Example 1: Quantitation limit solution: Take trifluoroethylamine reference substance and impurity reference substance, and prepare a solution containing 0.01 mg / mL of both trifluoroethylamine and trifluoroethanol with the diluent as the quantitation limit solution.

[0079] Detection limit solution: Take appropriate amounts of trifluoroethylamine reference substance and impurity reference substance, and prepare a solution containing 0.003 mg / mL of both trifluoroethylamine and trifluoroethanol with the diluent as the detection limit solution.

[0080] Detect the quantitation limit solution and detection limit solution by the above gas chromatography method, and calculate the quantitation limit and detection limit according to the signal-to-noise ratio. The results are shown in Table 9.

[0081] Table 9: Test results of quantitation limit and detection limit.

[0082] It can be seen from the results in Table 9 that when sodium hydroxide is not added to the diluent in Comparative Example 1, the quantitation limit and detection limit of trifluoroethylamine and trifluoroethanol cannot meet the requirements (the requirement is that the quantitation limit is not lower than 30% of the limit concentration, the detection limit is not lower than 10% of the limit, and the impurity limit is 0.1%).

[0083] The present invention uses a sodium hydroxide solution as a diluent. After the trifluoroethylamine in trifluoroethylamine hydrochloride is liberated with the sodium hydroxide solution, gas chromatography is used for detection, which can solve the problems of poor peak shape and baseline, and has good specificity, accuracy, detection limit and quantification limit; the system suitability meets the requirements. The method of the present invention is simple to operate and has strong generality, and can be used for the quality control and evaluation of trifluoroethylamine hydrochloride.

[0084] The above is only the preferred embodiment of the present invention, and does not impose any formal or substantial limitations on the present invention. It should be noted that for those of ordinary skill in the art in this technical field, without departing from the method of the present invention, several improvements and supplements can still be made, and these improvements and supplements should also be regarded as the protection scope of the present invention. Those skilled in the art, without departing from the spirit and scope of the present invention, when making some equivalent changes, modifications and evolutions using the technical content disclosed above, are all equivalent embodiments of the present invention; at the same time, any equivalent changes, modifications and evolutions made to the above embodiments based on the essential technology of the present invention still fall within the scope of the technical solution of the present invention.

Claims

1. A method for testing the impurity content in trifluoroethylamine hydrochloride, characterized in that: The steps include: (1) preparing sodium hydroxide solution as a diluent; (2) dissolving the trifluoroethylamine hydrochloride test sample and the reference sample in a diluent to obtain a test sample solution and a reference sample solution; (3) The test solution and the reference solution were sampled and tested by headspace gas chromatography, and the impurity content in trifluoroethylamine hydrochloride was calculated according to the main component external standard method.

2. The method for testing the impurity content in trifluoroethylamine hydrochloride according to claim 1, characterized in that: The concentration of the sodium hydroxide solution in step (1) is 0.09-0.11 g / mL.

3. The method for testing the impurity content in trifluoroethylamine hydrochloride according to claim 1, characterized in that: The concentration of the trifluoroethylamine hydrochloride test sample in the test solution in step (2) is 95-105 mg / mL.

4. The method for testing the impurity content in trifluoroethylamine hydrochloride according to claim 1, characterized in that: The concentration of the trifluoroethylamine hydrochloride reference substance in the reference substance solution in step (2) is 0.08 to 0.12 mg / mL.

5. The method for testing the impurity content in trifluoroethylamine hydrochloride according to claim 1, characterized in that: The gas chromatography conditions in step (3) include: starting temperature 40±2°C, maintaining for 4 to 6 minutes, heating to 55 to 65°C at a rate of 5±1°C per minute, and then heating to 240 to 245°C at a rate of 40±5°C per minute, and maintaining for 4 to 6 minutes.

6. The method for testing the impurity content in trifluoroethylamine hydrochloride according to claim 1 or 5, characterized in that: The gas chromatography conditions in step (3) include: a column flow rate of 2 to 4 mL / min, a split ratio of 18 to 22:1; a capillary column with 4 to 6 wt% cyanopropylphenyl and 94 to 96 wt% polydimethylsiloxane as the stationary phase; an injection port temperature of 195 to 205° C., and nitrogen as the carrier gas.

7. The method for testing the impurity content in trifluoroethylamine hydrochloride according to claim 6, characterized in that: The capillary column is DB-624, with a length of 30 m, an inner diameter of 0.53 mm, and a film thickness of 3.0 μm.

8. The method for testing the impurity content in trifluoroethylamine hydrochloride according to claim 1 or 5, characterized in that: The headspace conditions of the gas chromatography in step (3) include: sample equilibrium temperature 80±2°C; transfer line temperature 100±2°C; quantitative loop temperature 90±2°C; headspace equilibrium time 28 to 32 minutes; and cycle time 20 to 30 minutes.

9. The method for testing the impurity content in trifluoroethylamine hydrochloride according to claim 1, characterized in that: The calculation formula for the impurity content in step (3) is: Where, As: peak area of ​​each impurity in the test solution; A R : The main component peak area of ​​the reference solution; W R : The weight of the reference substance, mg; W S : The weight of the test sample, mg; D R : Dilution multiple of reference solution; D S : dilution factor of the sample; P: The content of the main component in the reference substance.

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