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Method for detecting triethylamine and N, N-diethylaniline in ceftazidime and application

A technology of diethylaniline and ceftazidime, which can be used in measurement devices, instruments, scientific instruments, etc., can solve the problem of limited types of residual solvents, and achieve the effects of good system adaptability, good linearity, and good accuracy

Pending Publication Date: 2022-04-29
武汉九州钰民医药科技有限公司
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  • 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 ceftazidime in the prior art, thereby providing a detection method and application of triethylamine and N,N-diethylaniline in ceftazidime

Method used

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  • Method for detecting triethylamine and N, N-diethylaniline in ceftazidime and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] (1) Chromatographic conditions:

[0050] Instrument: gas chromatograph (Shimadzu GC-2014C), detector is hydrogen flame ionization detector (FID);

[0051] Chromatographic column: CP-Volamine, 30m×0.32mm, 5.0μm or a capillary column with equivalent performance;

[0052] 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;

[0053] The inlet temperature is 230°C; the detector temperature is 250°C;

[0054] Column flow rate is 1.0mL / min

[0055] Blank solvent: dimethylsulfoxide.

[0056] (2) Solution preparation: See Table 1 for the solution preparation process.

[0057] Table 1 Triethylamine and N, N-diethylaniline solution preparation process

[0058]

[0059] The specific operation is as follows:

[0060] N,N-diethylaniline stock solution: Take 50mg of N,N-diethylaniline, put it in a 100mL measuring bottle, add dimethyl sulfoxide to dissolve and dilute to the...

Embodiment 2

[0092] Verification Example 2: Linearity and Range

[0093] (1) Test process:

[0094] The preparation process of the linear solution is shown in Table 7 (preparation process of the linear solution of triethylamine and N,N-diethylaniline). Precisely measure 1 μL of each linear solution, inject them into the gas chromatograph respectively, and record the chromatogram. 30% linear solution is limit of quantitation, as the starting point of linearity, with the concentration of each solution as abscissa, with each solvent peak area as ordinate to carry out linear regression (results see Figure 7 and Figure 8 ).

[0095] Table 7 Triethylamine and N, N-diethylaniline linear solution preparation process

[0096] linear solution Triethylamine concentration (μg / mL) N, N-diethylaniline concentration (μg / mL) prepare 30％ 150.00 1.50 Linear stock solution 3mL→20mL 40％ 200.00 2.00 Linear stock solution 2mL→10mL 60％ 300.00 3.00 Linear stock solutio...

Embodiment 3

[0112] Validation Example 3: Limits of Detection and Limits of Quantitation

[0113] (1) Test process:

[0114] Accurately measure the linear solution (limit 30%) 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.

[0115] (2) Results and conclusions:

[0116] Table 10 triethylamine, N, N-diethylaniline quantitative limit and detection limit results

[0117]

[0118] Table 11 Triethylamine, N, N-diethylaniline quantitative limit system precision results

[0119] Element 1 2 3 4 5 6 average RSD(%) Triethylamine 203956 204855 199872 200868 198898 198591 201173 1.32 ...

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Abstract

The invention discloses a method for detecting triethylamine and N, N-diethylaniline in ceftazidime 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 modified dimethyl polysiloxane 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 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 triethylamine and N, N-diethylaniline in ceftazidime. 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 standard...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/68
CPCG01N30/06G01N30/68
Inventor 姚萌霞刘均均龚丹凤张恒陈龙余艳平范昭泽胡仁军
Owner 武汉九州钰民医药科技有限公司
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