Method for detecting N-nitroso moxifloxacin in moxifloxacin hydrochloride sodium chloride injection
The content of N-nitrosomoxifloxacin in sodium chloride injection was detected by high-performance liquid chromatography-mass spectrometry, which solved the problem that the existing technology could not effectively control the impurity content, achieved high sensitivity and accuracy detection, and ensured product quality.
Patent Information
- Application Number
- CN202510109014.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-23
- Publication Date
- 2025-05-06
AI Technical Summary
The prior art has failed to effectively control the content of N-nitrosomoxifloxacin in sodium chloride injection, resulting in difficulty in ensuring product quality.
The content of N-nitrosomoxifloxacin was detected by high performance liquid chromatography-mass spectrometry. By providing the moxifloxacin hydrochloride solution to be tested and recording the chromatogram, the content of N-nitrosomoxifloxacin was calculated according to the specific formula.
The high sensitivity and accuracy of N-nitrosomoxifloxacin in sodium chloride injection has been achieved, which can effectively control the quality of the product and ensure that it meets the specified content limit.
Smart Images
Figure CN119936246A_ABST
Abstract
Description
Technical Field
[0001] The present application belongs to the technical field of drug analysis, and specifically relates to a method for detecting N-nitrosomoxifloxacin in moxifloxacin hydrochloride and sodium chloride injection. Background Art
[0002] Moxifloxacin hydrochloride sodium chloride injection, the main ingredient of which is moxifloxacin hydrochloride, chemical name: 1-cyclopropyl-7-[(S,S)-2,8-diazo-bicyclo[4.3.0]non-8-yl]-6-fluoro-8-methoxy-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid hydrochloride. Specification: 250 ml, 0.4 g moxifloxacin, 2.25 g sodium chloride. Moxifloxacin hydrochloride sodium chloride injection is a broad-spectrum fluoroquinolone antibacterial drug, mainly used to treat a variety of infections caused by sensitive bacteria.
[0003] N-nitrosomoxifloxacin, molecular formula: C 21 H 23 FN4O5, molecular weight: 430.44, its structural formula is as follows:
[0004]
[0005] It is a moxifloxacin impurity produced by the reaction of moxifloxacin hydrochloride and nitrite. According to ICH M7 and the Chinese Pharmacopoeia 2020 edition genotoxic impurity control guidelines, the main reference for determining the impurity limit is the acceptable daily intake. The calculation method includes: calculation based on compound-specific risk assessment, toxicological concern threshold and dosing cycle adjustment calculation, etc. The limit: shall not exceed 3.25ppm.
[0006] Although ChP2020 and USP-NF2024 currently include the quality standards for moxifloxacin hydrochloride raw materials, the pharmacopoeias of various countries do not include the quality standards for moxifloxacin hydrochloride sodium chloride injection, nor do they control N-nitrosomoxifloxacin.
[0007] Therefore, it is necessary to develop a detection method for N-nitrosomoxifloxacin in moxifloxacin hydrochloride and sodium chloride injection to control the content of the product in process production. Summary of the invention
[0008] In view of this, the primary purpose of the present application is to provide a method for detecting N-nitrosomoxifloxacin in moxifloxacin hydrochloride and sodium chloride injection, which adopts high performance liquid chromatography and mass spectrometry, and can effectively detect the content of N-nitrosomoxifloxacin in moxifloxacin hydrochloride and sodium chloride injection. The detection method is simple to operate, has good specificity, high sensitivity and accuracy, and can effectively control the quality of the product.
[0009] In order to achieve the above objectives, this application adopts the following technical solutions:
[0010] The present application provides a method for detecting N-nitrosomoxifloxacin in moxifloxacin hydrochloride and sodium chloride injection, wherein the method adopts high performance liquid chromatography-mass spectrometry and comprises the following steps:
[0011] Providing a moxifloxacin hydrochloride solution to be tested, wherein the moxifloxacin hydrochloride solution to be tested comprises a test solution and a reference solution;
[0012] Analyzing the moxifloxacin hydrochloride solution to be tested by high performance liquid chromatography-mass spectrometry, and recording a chromatogram of the moxifloxacin hydrochloride solution to be tested;
[0013] The content of N-nitrosomoxifloxacin was calculated according to the following formula:
[0014]
[0015] Where V 对 A is the dilution multiple of the reference solution; 对 is the peak area of N-nitrosomoxifloxacin in the reference solution; P 对 A is the purity or content of the reference solution; 供 V is the peak area of N-nitrosomoxifloxacin in the test solution; 供 is the dilution multiple of the test solution; m 对 is the sample weight of N-nitrosomoxifloxacin reference substance, mg; V0 is the sampling volume of the test substance, ml; filling volume is 250 ml, and the labeled amount is 0.4 g moxifloxacin.
[0016] In a further embodiment, in the HPLC-MS method, the HPLC conditions include a chromatographic column, wherein the chromatographic column uses octadecylsilane bonded silica gel as a filler, the filler particle size is 1.8 μm, the chromatographic column is 50 mm long, and the diameter is 2.1 mm.
[0017] In a further embodiment, in the HPLC-MS method, the HPLC conditions include column temperature, and the column temperature is 30°C.
[0018] In a further embodiment, in the HPLC-MS method, the HPLC conditions include a flow rate, and the flow rate is 0.3 ml / min.
[0019] In a further embodiment, in the HPLC-MS method, the HPLC conditions include an injection volume, and the injection volume is 1 μl.
[0020] In a further embodiment, in the HPLC-MS method, the HPLC conditions include a mobile phase, wherein the mobile phase includes a mobile phase A and a mobile phase B; the mobile phase A is a 0.01 mol / L aqueous solution of ammonium acetate, containing 0.1% by volume of formic acid; the mobile phase B is acetonitrile; the gradient elution is performed, and the elution procedure is as follows:
[0021]
[0022] .
[0024] In a further embodiment, in the high performance liquid chromatography-mass spectrometry method, the mass spectrometry conditions include: electrospray ionization ESI, using positive ion scanning mode; nozzle voltage 0V; nebulizer gas temperature 300°C; nebulizer gas flow rate 7L / min; sheath gas temperature 350°C; sheath gas flow rate 11L / min; nebulizer pressure 35psi; capillary voltage 3500V; scanning mode is multiple reaction ion scanning.
[0025] In a further embodiment, the test solution is prepared as follows:
[0026] Take an appropriate amount of this product and add water to quantitatively dilute it into a solution containing 0.4-0.8 mg of moxifloxacin per 1 ml;
[0027] Preferably, in the chromatogram of the test solution, if there is a chromatographic peak consistent with N-nitrosomoxifloxacin, the limit shall not exceed 3.25 ppm when calculated by peak area using the external standard method.
[0028] In a further embodiment, the reference solution is prepared as follows:
[0029] Take an appropriate amount of N-nitrosomoxifloxacin reference substance, accurately weigh it, add water to dilute it quantitatively, and prepare an N-nitrosomoxifloxacin stock solution containing 52 ng per 1 ml; then accurately measure the N-nitrosomoxifloxacin stock solution, add water to dilute it quantitatively, mix well, and prepare a reference substance solution with a concentration of 2.6 ng / ml.
[0030] In a further embodiment, the moxifloxacin hydrochloride solution to be tested further comprises a sensitivity solution, and in the chromatogram of the sensitivity solution, the signal-to-noise ratio of the chromatographic peak of N-nitrosomoxifloxacin should be no less than 10;
[0031] Preferably, the sensitivity solution is prepared as follows:
[0032] Take an appropriate amount of N-nitrosomoxifloxacin reference substance, accurately weigh it, add water to dilute it quantitatively, and prepare an N-nitrosomoxifloxacin stock solution containing 52 ng per 1 ml; then accurately measure the N-nitrosomoxifloxacin stock solution, add water to dilute it quantitatively, mix it well, and prepare a sensitivity solution with a concentration of 0.78 ng / ml.
[0033] Beneficial effects of this application:
[0034] The detection method of N-nitrosomoxifloxacin in moxifloxacin hydrochloride sodium chloride injection provided in the present application is simple to operate, short in analysis time, and the total analysis time is 13 minutes; the detection method has strong specificity; the recovery rate of the added sample solution is 81% to 89%, and the accuracy is good; the linear range is wide (0.773ng / ml to 5.154ng / ml), and within the linear range, the linear relationship is good; the sensitivity is high; the repeatability and solution stability are good.
[0035] In general, the detection method provided in this application can accurately determine the content of N-nitrosomoxifloxacin in the product and effectively control the quality of the product. BRIEF DESCRIPTION OF THE DRAWINGS
[0036] Figure 1 It is the chromatogram of the blank solvent (water) in Example 1.
[0037] Figure 2 The chromatogram of the test solution in Example 1.
[0038] Figure 3 It is the chromatogram of the reference substance solution in Example 1.
[0039] Figure 4 The chromatogram is of the sample solution added in Example 1.
[0040] Figure 5 It is the chromatogram of the sensitivity solution in Example 1.
[0041] Figure 6 It is the linear curve in Example 3. DETAILED DESCRIPTION
[0042] The following will clearly and completely describe the implementation methods of the present application. The technical solutions in the implementation methods described below are exemplary and are only possible technical implementations of the present application, not all possible implementations. Those skilled in the art can fully combine the implementation methods of the present application to obtain other implementation methods without creative work, and these implementation methods are also within the scope of protection of the present application.
[0043] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those commonly understood by those skilled in the art to which this application belongs. The terms used herein in the specification of this application are only for the purpose of describing specific embodiments and are not intended to limit this application.
[0044] In addition, unless otherwise specified, methods without specific conditions or steps are conventional methods, and the reagents and materials used are all commercially available.
[0045] The information of the products and reference substances involved in the following examples is as follows:
[0046]
[0047] Example 1
[0048] This example provides a method for detecting N-nitrosomoxifloxacin in moxifloxacin hydrochloride and sodium chloride injection using high performance liquid chromatography-mass spectrometry.
[0049] (1) High performance liquid chromatography-mass spectrometry (triple quadrupole): 1290 InfinityⅡ / G6470B.
[0050] (2) HPLC conditions:
[0051] The chromatographic column was filled with octadecylsilane bonded silica gel, Agilent ZORBAX Eclipse Plus C18 (2.1 × 50 mm, 1.8 μm);
[0052] The mobile phase includes mobile phase A and mobile phase B. Mobile phase A is 0.01 mol / L ammonium acetate aqueous solution (containing 0.1% formic acid by volume), and mobile phase B is acetonitrile. Gradient elution is performed. The elution procedure is as follows:
[0053] Time (min) Mobile phase A (%) Mobile phase B (%) 0 95 5 1 95 5 1.5 80 20 4 80 20 7 10 90 10 10 90 10.1 95 5 13 95 5
[0054] Injection volume: 1 μl; column temperature: 30°C; flow rate: 0.3 ml / min.
[0055] (3) Mass spectrometry conditions:
[0056] An electrospray ionization source (ESI) was used in positive ion scanning mode, with nozzle voltage of 0 V, nebulizer gas temperature of 300°C, nebulizer gas flow rate of 7 L / min, sheath gas temperature of 350°C, sheath gas flow rate of 11 L / min, nebulizer pressure of 35 psi, and capillary voltage of 3500 V; scanning mode was MRM (multiple reaction ion scanning).
[0057] Scan segments:
[0058]
[0059] Collection time segment:
[0060] Start Time Scan Type Div Valve Delta EMV+ Delta EMV- 0 MRM To MS 0 0 3.6 MRM To Waste 0 0 5.7 MRM To MS 0 0
[0061] (4) Solution preparation:
[0062] N-nitrosomoxifloxacin stock solution: Take an appropriate amount of N-nitrosomoxifloxacin reference substance, accurately weigh it, and add water to quantitatively dilute it to make a solution containing approximately 52 ng per 1 ml.
[0063] Sensitivity solution: Accurately add 15 μl of N-nitrosomoxifloxacin stock solution into a 1 ml volumetric flask, dilute to the mark with water, mix well, and prepare a solution with a concentration of 0.78 ng / ml.
[0064] Test solution: Take 0.5 ml of the product, place it in a 1 ml volumetric flask, add water to dilute to the scale, and mix well.
[0065] Reference solution: Accurately measure 50 μl of N-nitrosomoxifloxacin stock solution and place it in a 1 ml volumetric flask. Add water to dilute to the mark and mix well to prepare a solution with a concentration of 2.6 ng / ml.
[0066] Add the test solution: Take 0.5 ml of the product and place it in a 1 ml volumetric flask, accurately add 50 μl of N-nitrosomoxifloxacin stock solution, dilute to the scale with water, and mix well.
[0067] (5) Sample determination: After the system is stable, inject blank solvent, sensitivity solution, test solution, reference solution, and sampled test solution into the HPLC-MS instrument. The chromatograms of each solution are shown in Table 1. Figure 1-Figure 5 The detection and analysis results are shown in Table 1, where the signal-to-noise ratio of the N-nitrosomoxifloxacin peak in the sensitivity solution chromatogram should not be less than 10.
[0068] Table 1 Detection and analysis results of each solution in Example 1
[0069] name Peak name Retention time (min) Peak area A Signal-to-Noise Ratio (S / N) Blank solvent (water) -- -- -- -- Sensitivity solution N-nitrosomoxifloxacin 6.606 753 105.9 Test solution N-nitrosomoxifloxacin 6.613 452 -- Reference solution N-nitrosomoxifloxacin 6.606 2911 -- Add test solution N-nitrosomoxifloxacin 6.606 3073 --
[0070] In this example, the specificity of the detection method was investigated by adding known impurities. Figure 1-Figure 5 The results in Table 1 show that the detection method has no interference with the detection of N-nitrosomoxifloxacin and has good method specificity.
[0071] Example 2 Accuracy Experiment
[0072] (1) The HPLC-MS instrument, HPLC conditions and mass spectrometry conditions were all the same as those in Example 1.
[0073] (2) The solution is prepared as follows:
[0074] N-nitrosomoxifloxacin stock solution: Take an appropriate amount of N-nitrosomoxifloxacin reference substance, accurately weigh it, and add water to quantitatively dilute it to make a solution containing approximately 52 ng per 1 ml.
[0075] Reference solution: Accurately add 50 μl of N-nitrosomoxifloxacin stock solution, place in a 1 ml volumetric flask, dilute to the mark with water, mix well, and prepare a solution with a concentration of 2.6 ng / ml.
[0076] Sample-spike test solution: Take 0.5 ml of this product and place it in 1 ml volumetric bottles, accurately add 15 μl, 50 μl, and 75 μl of N-nitrosomoxifloxacin stock solution, dilute to the mark with water, mix well, and use them as sample-spike test solutions with limit concentration of 30%, limit concentration (3.25 ppm), and limit concentration of 150%, respectively. Prepare three replicates of sample-spike test solutions at each concentration level.
[0077] (3) Sample determination: After the system is stabilized, sample solutions are injected into the HPLC-MS / MS instrument. The test results are shown in Table 2.
[0078] Table 2 Accuracy experimental results
[0079]
[0080]
[0081] It can be seen from the test results in Table 2 that the recoveries of the test solution at 30% limit, limit concentration, and limit concentration of 150% were between 81% and 89%, and in the range of 70% to 130%, the RSDs (n=9) were 3.1%, respectively, all of which were no more than 20.0%, indicating that the detection method of the present application has good accuracy.
[0082] Example 3 Linearity Experiment
[0083] (1) The HPLC-MS instrument, HPLC conditions and mass spectrometry conditions were all the same as those in Example 1.
[0084] (2) The solution is prepared as follows:
[0085] N-nitrosomoxifloxacin stock solution: Take an appropriate amount of N-nitrosomoxifloxacin reference substance, accurately weigh it, and add water to quantitatively dilute it to make a solution containing approximately 52 ng per 1 ml.
[0086] Linear solutions 1-5: Accurately measure 15μl, 25μl, 30μl, 50μl, 75μl, and 100μl of N-nitrosomoxifloxacin stock solution, place them in 1ml volumetric flasks respectively, dilute to the scale with water, and shake well.
[0087] (3) Sample determination: After the system is stable, take linear solutions 1 to 5 and inject them into the HPLC-MS / MS instrument. The linear curve is shown in Figure 6 , the test results are shown in Table 3.
[0088] Table 3 Linearity test results
[0089]
[0090] pass Figure 6 The results in Table 3 show that the detection method of the present application has a good linear relationship in the range of 0.773 ng / ml to 5.154 ng / ml, and can quantitatively detect the content of N-nitrosomoxifloxacin.
[0091] Example 4 Repeatability Experiment
[0092] (1) The HPLC-MS instrument, HPLC conditions and mass spectrometry conditions were all the same as those in Example 1.
[0093] (2) Solution preparation:
[0094] The limit concentration (3.25 ppm) test solution was prepared according to the method in the accuracy experiment in Example 2, and six replicates were prepared in parallel to examine the repeatability.
[0095] (3) Sample determination: After the system is stable, six portions of the limit concentration (3.25 ppm) of the test solution are taken and injected into the HPLC-MS / MS instrument. The test results are shown in Table 4.
[0096] Table 4 Repeatability experiment
[0097]
[0098] The results in Table 4 show that the RSD of the N-nitrosomoxifloxacin content in the 6 sample solutions is less than 15%, indicating that the detection method of the present application has good repeatability.
[0099] Example 5 Solution stability test
[0100] (1) The HPLC-MS instrument, HPLC conditions and mass spectrometry conditions were all the same as those in Example 1.
[0101] (2) Solution preparation:
[0102] The reference solution and the test solution with the limit concentration (3.25 ppm) were prepared by referring to the method in the accuracy experiment in Example 2, and placed at room temperature. Samples were taken and measured at different time points to examine the stability of the solution.
[0103] (3) Sample determination: After the system is stable, sample solutions of the limit concentration (3.25 ppm) at different time points are taken and injected into the HPLC-MS / MS instrument. The test results are shown in Table 5.
[0104] Table 5 Solution stability test results
[0105]
[0106] The results in Table 5 show that the RSD of the peak areas of the reference solution and the sampled test solution at different time points at room temperature are all less than 20.0%, indicating that the reference solution and the sampled test solution are stable within 12 hours at room temperature.
[0107] Example 6 Quantitative Limit Detection Limit Experiment
[0108] (1) The HPLC-MS instrument, HPLC conditions and mass spectrometry conditions were all the same as those in Example 1.
[0109] (2) Solution preparation:
[0110] Take an appropriate amount of N-nitrosomoxifloxacin reference substance and dilute it with water to make solutions with concentrations of 0.258 ng / ml and 0.773 ng / ml, which are used as the detection limit solution (LOD) and quantification limit solution (LOQ), respectively.
[0111] (3) Sample determination: After the system is stable, the samples are injected into the HPLC-MS / MS instrument. The detection limit solution is continuously determined for 3 times, and the quantification limit solution is continuously determined for 6 times. The test results are shown in Table 6.
[0112] Table 6 Quantitative limit and detection limit experimental results
[0113]
[0114] It can be seen from the results in Table 6 that the detection method of the present application has good sensitivity, can effectively control the content of N-nitrosomoxifloxacin, eliminate potential medication risks, and ensure the effectiveness and safety of drug quality.
[0115] Example 7 Detection of different batches of samples
[0116] (1) The HPLC-MS instrument, HPLC conditions and mass spectrometry conditions were all the same as those in Example 1.
[0117] (2) Solution preparation:
[0118] Test solution: Take an appropriate amount of this product and dilute it quantitatively with water to make a solution containing approximately 0.8 mg of moxifloxacin per 1 ml.
[0119] Reference solution: Take an appropriate amount of N-nitrosomoxifloxacin reference substance, weigh accurately, dissolve in water and quantitatively dilute to make a solution containing approximately 2.6 ng of N-nitrosomoxifloxacin per 1 ml.
[0120] Sensitivity solution: Take an appropriate amount of N-nitrosomoxifloxacin reference substance, weigh accurately, dissolve in water and quantitatively dilute to make a solution containing approximately 0.78 ng of N-nitrosomoxifloxacin per 1 ml.
[0121] (3) After the system is stable, take the test sample and inject it into the high performance liquid chromatography-mass spectrometer, and calculate according to the following formula:
[0122]
[0123] Where:
[0124] V 对 : Dilution multiple of reference substance;
[0125] A 对 : N-nitrosomoxifloxacin peak area in reference solution;
[0126] P 对 : Purity / content of reference solution;
[0127] A 供 : N-nitrosomoxifloxacin peak area in the test solution;
[0128] V 供 : Dilution multiple of the test sample.
[0129] m 对 : Sample weight of N-nitrosomoxifloxacin reference substance, mg.
[0130] V0: sampling volume of the test sample, ml.
[0131] Filling volume 250ml, labeled amount 0.4g (moxifloxacin)
[0132] Limit: If there is a chromatographic peak consistent with N-nitrosomoxifloxacin in the chromatogram of the test solution, the peak area calculated by the external standard method shall not exceed 3.25 ppm.
[0133] The test results are shown in Table 7.
[0134] Table 7 Test results of multiple batches of samples
[0135]
[0136] The results in Table 7 show that the content of N-nitrosomoxifloxacin in the three batches of samples meets the requirements.
[0137] It should be noted that the present application is not limited to the above-mentioned embodiments. The above-mentioned embodiments are only examples, and the embodiments having the same structure as the technical idea and exerting the same effect within the scope of the technical solution of the present application are all included in the technical scope of the present application. In addition, without departing from the scope of the main purpose of the present application, various modifications that can be thought of by those skilled in the art to the embodiments and other methods of combining some of the constituent elements in the embodiments are also included in the scope of the present application.
Claims
1. A method for detecting N-nitrosomoxifloxacin in moxifloxacin hydrochloride and sodium chloride injection, characterized in that: The detection method adopts high performance liquid chromatography-mass spectrometry detection, and comprises the following steps: Providing a moxifloxacin hydrochloride solution to be tested, wherein the moxifloxacin hydrochloride solution to be tested comprises a test solution and a reference solution; Analyzing the moxifloxacin hydrochloride solution to be tested by high performance liquid chromatography-mass spectrometry, and recording a chromatogram of the moxifloxacin hydrochloride solution to be tested; The content of N-nitrosomoxifloxacin was calculated according to the following formula: Where V 对 A is the dilution multiple of the reference solution; 对 is the peak area of N-nitrosomoxifloxacin in the reference solution; P 对 A is the purity or content of the reference solution; 供 V is the peak area of N-nitrosomoxifloxacin in the test solution; 供 is the dilution multiple of the test solution; m 对 is the sample weight of N-nitrosomoxifloxacin reference substance, mg; V0 is the sampling volume of the test substance, ml; filling volume is 250 ml, and the labeled amount is 0.4 g moxifloxacin.
2. The method for detecting N-nitrosomoxifloxacin in moxifloxacin hydrochloride and sodium chloride injection according to claim 1, characterized in that: In the HPLC-MS method, the HPLC conditions include a chromatographic column, wherein the chromatographic column uses octadecylsilane bonded silica gel as a filler, the filler particle size is 1.8 μm, the chromatographic column is 50 mm long, and the diameter is 2.1 mm.
3. The method for detecting N-nitrosomoxifloxacin in moxifloxacin hydrochloride and sodium chloride injection according to claim 1, characterized in that: In the HPLC-MS method, the HPLC conditions include column temperature, and the column temperature is 30°C.
4. The method for detecting N-nitrosomoxifloxacin in moxifloxacin hydrochloride and sodium chloride injection according to claim 1, characterized in that: In the HPLC-MS method, the HPLC conditions include a flow rate, and the flow rate is 0.3 ml / min.
5. The method for detecting N-nitrosomoxifloxacin in moxifloxacin hydrochloride and sodium chloride injection according to claim 1, characterized in that: In the HPLC-MS method, the HPLC conditions include the injection volume, and the injection volume is 1 μl.
6. The method for detecting N-nitrosomoxifloxacin in moxifloxacin hydrochloride and sodium chloride injection according to claim 1, characterized in that: In the HPLC-MS method, the HPLC conditions include a mobile phase, wherein the mobile phase includes a mobile phase A and a mobile phase B; the mobile phase A is a 0.01 mol / L ammonium acetate aqueous solution containing 0.1% by volume of formic acid; the mobile phase B is acetonitrile; the gradient elution is performed, and the elution procedure is as follows:
7. The method for detecting N-nitrosomoxifloxacin in moxifloxacin hydrochloride and sodium chloride injection according to claim 1, characterized in that: In the high performance liquid chromatography-mass spectrometry method, the mass spectrometry conditions include: electrospray ionization ESI, using positive ion scanning mode; nozzle voltage 0V; nebulizer gas temperature 300°C; nebulizer gas flow rate 7L / min; sheath gas temperature 350°C; sheath gas flow rate 11L / min; nebulizer pressure 35psi; capillary voltage 3500V; scanning mode is multiple reaction ion scanning.
8. The method for detecting N-nitrosomoxifloxacin in moxifloxacin hydrochloride and sodium chloride injection according to claim 1, characterized in that: The test solution was prepared as follows: Take an appropriate amount of this product and add water to quantitatively dilute it into a solution containing 0.4-0.8 mg of moxifloxacin per 1 ml; Preferably, in the chromatogram of the test solution, if there is a chromatographic peak consistent with N-nitrosomoxifloxacin, the limit shall not exceed 3.25 ppm when calculated by peak area using the external standard method.
9. The method for detecting N-nitrosomoxifloxacin in moxifloxacin hydrochloride and sodium chloride injection according to claim 1, characterized in that: The reference solution was prepared as follows: Take an appropriate amount of N-nitrosomoxifloxacin reference substance, accurately weigh it, add water to dilute it quantitatively, and prepare an N-nitrosomoxifloxacin stock solution containing 52 ng per 1 ml; then accurately measure the N-nitrosomoxifloxacin stock solution, add water to dilute it quantitatively, mix well, and prepare a reference substance solution with a concentration of 2.6 ng / ml.
10. The method for detecting N-nitrosomoxifloxacin in moxifloxacin hydrochloride and sodium chloride injection according to claim 1, characterized in that: The moxifloxacin hydrochloride solution to be tested also includes a sensitivity solution, and in the chromatogram of the sensitivity solution, the signal-to-noise ratio of the chromatographic peak of N-nitrosomoxifloxacin should be not less than 10; Preferably, the sensitivity solution is prepared as follows: Take an appropriate amount of N-nitrosomoxifloxacin reference substance, accurately weigh it, add water to dilute it quantitatively, and prepare an N-nitrosomoxifloxacin stock solution containing 52 ng per 1 ml; then accurately measure the N-nitrosomoxifloxacin stock solution, add water to dilute it quantitatively, mix it well, and prepare a sensitivity solution with a concentration of 0.78 ng / ml.