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Method for detecting benzene in ceftazidime residual solvent and application

A ceftazidime and residual solvent technology, which is applied to the detection and application field of benzene in ceftazidime residual solvent, can solve the problems of unloaded residual solvent detection methods and standards, and achieve the effects of good system adaptability, good specificity and good linearity

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

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Problems solved by technology

[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 included the quality standards of ceftazidime, but none of them included the detection methods and standards for residual solvents

Method used

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  • Method for detecting benzene in ceftazidime residual solvent and application
  • Method for detecting benzene in ceftazidime residual solvent and application
  • Method for detecting benzene in ceftazidime residual solvent and application

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Experimental program
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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-1, 30m×0.32mm, 1.0μm or equivalent capillary column;

[0054] Column temperature: the initial temperature is 50°C, maintain for 3 minutes, increase the temperature to 200°C at a rate of 10°C per minute, and maintain for 2 minutes;

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

[0056] The headspace equilibrium temperature is 90°C, and the equilibrium time is 30 minutes;

[0057] Air flow: 400mL / min; Hydrogen flow: 40mL / min; Column flow: 1.0mL / min;

[0058] Quantitative loop temperature: 140°C; transfer line temperature: 140°C;

[0059] Blank solvent: water.

[0060] (2) Solution preparation:

[0061] Table 1 Benzene solution preparation process

[0062]

[0063]

[0064] The specific operation is as follows:

[0065] The test ...

Embodiment 2

[0094] Verification Example 2: Linearity and Range

[0095] (1) Test process:

[0096] The preparation process of the linear solution is shown in Table 6 below (the preparation process of the benzene linear solution). Precisely measure 2 mL of the solution, put them into 20 mL headspace bottles, seal the cap, and inject the headspace sample. The linear solution (limit 10%) is the limit of quantification, and as the starting point of linearity, the concentration of each solution is taken as the abscissa, and the peak area of ​​each solvent is used as the ordinate to carry out linear regression (see figure 2 ).

[0097] Table 6 Preparation process of benzene linear solution

[0098]

[0099]

[0100] The specific operation is as follows:

[0101] Linear stock solution: Take 20mg of benzene, put it in a 20mL measuring bottle, add N,N-dimethylacetamide to dissolve and dilute to the mark, shake well, quantitatively dilute with water to make a solution containing 0.4μg per...

Embodiment 3

[0114] Validation Example 3: Limits of Detection and Limits of Quantitation

[0115] (1) Test process:

[0116] 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.

[0117] (2) Results and conclusions:

[0118] Table 8 Benzene quantitative limit and detection limit results

[0119]

[0120] Table 9 Benzene Quantitative Limit System Precision Results

[0121] Element 1 2 3 4 5 6 average RSD(%) benzene 972 846 902 986 985 1060 959 7.78

[0122] Table 10 Benzene quantitative limit recovery test result

[0123]

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Abstract

The invention discloses a method for detecting benzene in a ceftazidime residual solvent and application. The detection method disclosed by the invention comprises the following steps: respectively injecting a test solution and a reference solution into a gas chromatograph by adopting headspace sampling, recording a chromatogram, and carrying out quantitative analysis on the chromatogram by adopting an external standard method, wherein the detection conditions of the chromatography are as follows: a chromatographic column is a capillary column taking 100% dimethyl polysiloxane as a stationary liquid or a capillary chromatographic column with equivalent efficiency; the column temperature is programmed temperature rise: the initial temperature is 45-55 DEG C, the temperature is maintained for 3 minutes, and the temperature is raised to 200 DEG C at the rate of 10 DEG C per minute, and the temperature is maintained for 2 minutes; the balance temperature of the headspace bottle is 90 DEG C, and the balance time is 30 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 benzene 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 ceftazidime and anhydrous sodium carbonate, and organic solvents such as methanol and acetone are used in its production. Considering that there may be residual benzene in methanol and acetone, since the residual solvent is an impurity harmful to the human body in the drug, its 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...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/68
CPCG01N30/06G01N30/68Y02A50/30
Inventor 姚萌霞刘均均张璐胥红梅陈程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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