Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Method for detecting N, N-dimethylformamide in ceftazidime residual solvent and application

A technology of dimethylformamide and ceftazidime, applied to N in the residual solvent of ceftazidime, can solve the problem of limited types of residual solvents, and achieve the effects of good system adaptability, good linearity and good specificity

Pending Publication Date: 2022-05-06
武汉九州钰民医药科技有限公司
View PDF0 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to overcome the problem of limited types of residual solvents in the detection of ceftazime in the prior art, thereby providing a detection method and application of N, N-dimethylformamide in the residual solvent of ceftazidime

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for detecting N, N-dimethylformamide in ceftazidime residual solvent and application
  • Method for detecting N, N-dimethylformamide in ceftazidime residual solvent and application
  • Method for detecting N, N-dimethylformamide in ceftazidime residual solvent and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] (1) Chromatographic conditions:

[0052] Instrument: high-efficiency gas chromatograph (Shimadzu GC-2014C), the detector is a hydrogen flame ionization detector (FID);

[0053] Chromatographic column: DB-WAXETR, 30m×0.53mm, 2.0μm or equivalent capillary column;

[0054] Column temperature: the initial temperature is 100°C, maintained for 3 minutes, and raised to 220°C at a rate of 10°C per minute, maintained for 10 minutes;

[0055] The inlet temperature is 230°C; the detector temperature is 250°C;

[0056] Injection volume: 1μL; column flow: 3.0mL / min;

[0057] Air flow: 400mL / min; hydrogen flow: 40mL / min; split ratio: 5:1.

[0058] (2) Solution preparation: the solution preparation process is shown in Table 1

[0059] Table 1 Solution preparation

[0060]

[0061] The specific operation is as follows:

[0062] Reference substance stock solution: Take 88mg of N,N-dimethylformamide, put it in a 10mL measuring bottle, add dimethyl sulfoxide to dissolve and dilut...

Embodiment 2

[0089] Verification Example 2: Linearity and Range

[0090] (1) Test process:

[0091] The linear solution preparation process is shown in Table 5 (N,N-dimethylformamide linear solution preparation process). Precisely measure 1 μL of each linear solution, inject them into the gas chromatograph, and record the chromatogram. The linear solution (10% linear solution) is the limit of quantification, as the starting point of linearity, the concentration of each solution is the abscissa, and the peak area of ​​each solvent is the ordinate to carry out linear regression (results are shown in figure 2 ).

[0092] Table 5 N, N-dimethylformamide linear solution preparation process

[0093] linear solution Concentration (μg / mL) prepare 10％ 8.80 Linear stock solution 1mL→20mL 20％ 17.60 Linear stock solution 1mL→10mL 40％ 35.20 Linear stock solution 2mL→10mL 60％ 52.80 Linear stock solution 3mL→10mL 100％ 88.00 Linear stock solution 5mL→10mL...

Embodiment 3

[0107] Validation Example 3: Limits of Detection and Limits of Quantitation

[0108] (1) Test process:

[0109] Accurately measure the linear solution (limit 10%) under "Verification Example 2: Linearity and Range", the signal-to-noise ratio (S / N) is greater than 10:1, which can be used as the limit of quantification. Dilute the limit of quantitation, according to the signal-to-noise ratio (S / N) greater than 3:1, can be used as the detection limit. The quantitative limit was injected 6 times continuously, the peak area was recorded, and the average value and RSD value were calculated.

[0110] (2) Results and conclusions:

[0111] Table 7 N, N-dimethylformamide quantitative limit and detection limit results

[0112]

[0113] Table 8 N, N-dimethylformamide quantitative limit system precision results

[0114] Element 1 2 3 4 5 6 average RSD(%) N,N-Dimethylformamide 6509 6810 6622 6545 6509 6491 6581 1.85

[0115] Table 9 N, N-dimethyl...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a method for detecting N, N-dimethylformamide in a ceftazidime residual solvent and application of the method. The detection method disclosed by the invention comprises the following steps: injecting a test solution containing ceftazidime into a gas chromatograph in a direct sample injection manner, recording a chromatogram, and calculating the content according to an external standard method; wherein the detection conditions of the chromatography are as follows: a chromatographic column is a capillary column taking polyethylene glycol as a stationary liquid or a capillary chromatographic column with equivalent efficiency; the initial temperature is 95-105 DEG C, the temperature is maintained for 3 minutes, the temperature is raised to 220 DEG C at the rate of 10 DEG C per minute, and the temperature is maintained for 10 minutes; the sample size is 1 microliter. The method has good specificity and system adaptability, extremely low detection limit and quantitation limit, good linearity and good accuracy.

Description

technical field [0001] The invention relates to a detection method and application of N,N-dimethylformamide in ceftazidime residual solvent. Background technique [0002] Ceftazidime is a semi-synthetic third-generation cephalosporin antibiotic, which belongs to the β-lactam antibiotics and has good antibacterial effects on both Gram-negative bacteria and Gram-positive bacteria. [0003] Ceftazidime (containing sodium carbonate) raw material is a mixed powder of ceftazime and anhydrous sodium carbonate, and organic solvents are used in its production. Considering the harm of organic solvents to the human body and the possibility of residual solvents used in the product, their content should be controlled within the limit during the production process. [0004] The 43rd edition of the United States Pharmacopoeia, the 10.0th edition of the European Pharmacopoeia, the 2020 edition of the British Pharmacopoeia, and the 2020 Chinese Pharmacopoeia only include the quality standar...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): G01N30/06G01N30/68
CPCG01N30/06G01N30/68
Inventor 刘均均姚萌霞苏立林岳翎王菲菲余艳平范昭泽胡仁军
Owner 武汉九州钰民医药科技有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com