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CN-122017066-A - Levofloxacin dimethylamine detection method

CN122017066ACN 122017066 ACN122017066 ACN 122017066ACN-122017066-A

Abstract

The invention discloses a method for detecting dimethylamine in levofloxacin, which comprises the following steps of weighing levofloxacin, adding a diluent for dissolution and dilution, taking filtrate to obtain a sample solution, taking a dimethylamine hydrochloride reference substance, adding the diluent for dissolution and dilution to obtain a reference substance solution, taking the reference substance solution and the sample solution, respectively injecting the reference substance solution and the sample solution into an ion chromatograph, recording a chromatogram, and calculating by a peak area according to an external standard method to obtain the dimethylamine content. According to the method for detecting the dimethylamine in the levofloxacin, provided by the invention, the content of the dimethylamine in the levofloxacin is measured by the ion chromatography, the method is simple, convenient and feasible, the specificity is strong, the accuracy is high, the repeatability is good, the detection sensitivity is high, and the content of the dimethylamine in the levofloxacin raw material can be accurately and sensitively detected, so that the quality of the levofloxacin raw material is ensured.

Inventors

  • JIANG LU
  • FANG FANG
  • XU HANG
  • HUANG PING
  • ZHU JUN
  • YU LIUYING

Assignees

  • 湖南科伦制药有限公司

Dates

Publication Date
20260512
Application Date
20260204

Claims (9)

  1. 1. The method for detecting dimethylamine in levofloxacin is characterized by comprising the following steps of: Weighing levofloxacin, adding a diluent for dissolution and dilution, and taking filtrate to obtain a sample solution; Taking dimethylamine hydrochloride reference substance, adding a diluent for dissolution and dilution to obtain a reference substance solution; And (3) taking the reference substance solution and the sample solution, respectively injecting into an ion chromatograph, recording a chromatogram, and calculating according to an external standard method and peak area to obtain the dimethylamine content.
  2. 2. The method for detecting dimethylamine in levofloxacin according to claim 1, wherein the diluent is 0.01mol/L methane sulfonic acid solution.
  3. 3. The method for detecting dimethylamine in levofloxacin according to claim 2, wherein the analytical column of the ion chromatograph is a cation exchange column, the detector of the ion chromatograph is a conductivity detector, and the detection mode of the ion chromatograph is inhibition conductivity detection.
  4. 4. The method for detecting dimethylamine in levofloxacin according to claim 3, wherein the size of the analytical column of the ion chromatograph is 5mm by 250mm and the size of the guard column is 4mm by 50mm.
  5. 5. The method for detecting dimethylamine in levofloxacin according to claim 4, wherein the chromatographic conditions of the ion chromatograph are that the column temperature of the analytical column is 35 ℃, the flow rate is 0.98-1.02ml/min, the sample injection amount is 25 μl, and the eluent is methane sulfonic acid solution.
  6. 6. The method for detecting dimethylamine in levofloxacin according to claim 5, wherein the gradient elution mode of the eluent is that the concentration of the eluent is 0.017 to 0.023mol/L for 0 to 30.0min, the concentration of the eluent is 0.035mol/L for 30.0 to 30.1min, the concentration of the eluent is kept at 0.035mol/L for 30.1 to 40.0min, the concentration of the eluent is kept at 0.02mol/L for 40.0 to 40.1min, and the concentration of the eluent is kept at 0.02mol/L for 40.1 to 50.0 min.
  7. 7. The method for detecting dimethylamine in levofloxacin according to claim 6, wherein the gradient elution mode of the eluent is that the concentration of the eluent is 0.02mol/L in 0-30.0min, the concentration of the eluent is 0.035mol/L in 30.0-30.1min, the concentration of the eluent is kept 0.035mol/L in 30.1-40.0min, the concentration of the eluent is kept 0.02mol/L in 40.0-40.1min, and the concentration of the eluent is kept 0.02mol/L in 40.1-50.0 min.
  8. 8. The method for detecting dimethylamine in levofloxacin according to claim 7, wherein the flow rate of the eluent is 1.0ml/min.
  9. 9. The method for detecting dimethylamine in levofloxacin according to claim 8, wherein the dimethylamine calculation formula is: (1) (2) (3) (4) Wherein, the A Ti is the peak area of the ion to be detected in the sample solution; a Si is the peak area of the ion to be detected in the reference substance solution; D S is the dilution factor of the control solution; d T is the dilution of the sample solution; W Si is the weighing of the reference substance; w Ti is the weighing of the sample; 1 and 2 Are respectively correction factors of the reference substance solution; is an average correction factor; W1 and W2 are the contents of the to-be-detected objects respectively; The average content of the object to be detected; p is the purity of the reference substance; F is the conversion coefficient of dimethylamine and dimethylamine hydrochloride.

Description

Levofloxacin dimethylamine detection method Technical Field The invention relates to the field of anesthetic production, in particular to a method for detecting dimethylamine in levofloxacin. Background Levofloxacin is one of quinolone medicines, has broad-spectrum antibacterial effect and strong antibacterial effect, and has strong antibacterial activity on most enterobacteriaceae bacteria such as escherichia coli, klebsiella, proteus, salmonella, shigella, haemophilus influenzae, legionella pneumophila, neisseria gonorrhoeae and other gram-negative bacteria. Clinically used as a core medicine for treating respiratory tract infection, genitourinary system infection and the like. The levofloxacin is easy to produce by-product dimethylamine in the synthesis process, and the dimethylamine has strong damage to skin, eye mucosa and the like and has strong irritation to respiratory tract. At present, no method for detecting the content of dimethylamine in levofloxacin is reported in pharmacopoeias and documents of various countries, wherein the prior patent (patent publication No. CN115616119A, patent name: detection method of dimethylamine in levofloxacin) adopts a derivatization high performance liquid chromatography to detect dimethylamine, but the patent needs to adopt a plurality of derivatization reagents such as sodium tetraborate decahydrate solution, 9-fluorenylmethyl chloroformate solution, citric acid solution and the like for derivatization, the operation is relatively complex, and acetonitrile and other organic solvents are needed, and the waste liquid treatment cost is high. Therefore, a method for detecting dimethylamine in levofloxacin is needed. Disclosure of Invention The invention aims to provide a method for detecting dimethylamine in levofloxacin, which adopts ion chromatography to detect dimethylamine, is accurate and sensitive and has higher safety. The invention provides a method for detecting dimethylamine in levofloxacin, which comprises the following steps: Weighing levofloxacin, adding a diluent for dissolution and dilution, and taking filtrate to obtain a sample solution; Taking dimethylamine hydrochloride reference substance, adding a diluent for dissolution and dilution to obtain a reference substance solution; And (3) taking the reference substance solution and the sample solution, respectively injecting into an ion chromatograph, recording a chromatogram, and calculating according to an external standard method and peak area to obtain the dimethylamine content. In the method for detecting dimethylamine in levofloxacin, preferably, the diluent is 0.01mol/L methane sulfonic acid solution. In the method for detecting dimethylamine in levofloxacin, preferably, the analysis column of the ion chromatograph is a cation exchange column, the detector of the ion chromatograph is a conductivity detector, and the detection mode of the ion chromatograph is to inhibit conductivity detection. In the method for detecting dimethylamine in levofloxacin, preferably, the size of the analysis column of the ion chromatograph is 5mm×250mm, and the size of the protection column is 4mm×50mm. In the method for detecting dimethylamine in levofloxacin, preferably, the chromatographic conditions of the ion chromatograph are that the column temperature of the analysis column is 35 ℃, the flow rate is 0.98-1.02ml/min, the sample injection amount is 25 μl, and the eluent is methane sulfonic acid solution. In the method for detecting dimethylamine in levofloxacin, preferably, the gradient elution mode of the eluent is that the concentration of the eluent is 0.017-0.023mol/L for 0-30.0min, the concentration of the eluent is 0.035mol/L for 30.0-30.1min, the concentration of the eluent is kept at 0.035mol/L for 30.1-40.0min, the concentration of the eluent is kept at 0.02mol/L for 40.0-40.1min, and the concentration of the eluent is kept at 0.02mol/L for 40.1-50.0 min. In the method for detecting dimethylamine in levofloxacin, preferably, the gradient elution mode of the eluent is that the concentration of the eluent is 0.02mol/L in 0-30.0min, the concentration of the eluent is 0.035mol/L in 30.0-30.1min, the concentration of the eluent is kept 0.035mol/L in 30.1-40.0min, the concentration of the eluent is kept 0.02mol/L in 40.0-40.1min, and the concentration of the eluent is kept 0.02mol/L in 40.1-50.0 min. In the method for detecting dimethylamine in levofloxacin, preferably, the flow rate of the leaching solution is 1.0ml/min. In the method for detecting dimethylamine in levofloxacin, preferably, the dimethylamine calculation formula is as follows: (1) (2) (3) (4) Wherein, the A Ti is the peak area of the ion to be detected in the sample solution; a Si is the peak area of the ion to be detected in the reference substance solution; D S is the dilution factor of the control solution; d T is the dilution of the sample solution; W Si is the weighing of the reference substance; w Ti is the weighing of the sample; 1 a