I am honored to recommend it to youAnalysis of Residual Solvent Content in Cefotaxime Sodium by Gas ChromatographyThe determination of residual solvent content in cefotaxime sodium by gas chromatography is one of the key research and development products of Tengzhou Zhongke Spectral Analysis Instrument Co., Ltd. If you have any needs or suggestions, please feel free to contact us at:, and we will be happy to serve you!

Cefotaxime sodium is a third-generation broad-spectrum cephalosporin antibiotic widely used in clinical practice. The quality directly affects the clinical efficacy. Therefore, rapid and accurate detection of product quality is an effective means to ensure high-quality products. In accordance with the standards of the pharmacopoeia, we are exploring the establishment of a new, simple, and accurate gas chromatography method for the determination of residual solvents in the synthesis of cefotaxime sodium produced by our factory. This method can quickly and effectively detect residual solvents and is worth promoting.

1 Experimental section

1.1 Experimental instrument: ZhongkepuGC-2010Gas chromatograph:FIDdetector;Chromatographic column:HP-FFAP（Cross linked polyethylene glycol-TPA，25em×0.25mm×0.25μm（Film thickness）.

1.2 Reagents: Ethyl acetate, tetrahydrofuran, isopropanol are chromatographically pure（Shanghai Institute of Chemical Reagents）All water used in the experiment is double distilled water（Chromatographic analysis shows no interference peaks）.

1.3 Chromatographic conditions: Nitrogen as carrier gas, column pressure100Kpa, diversion ratio200：1, detector temperature250℃ , Injection port temperature200℃ Column temperature（Using programmed heating）Initial temperature55℃ , Reserved1.7minAnd then30℃/minThe rate of increase90℃ , Reservedlmin.

2 sample determination

2.1 Preparation of internal standard solution and reference solution: Take1.0mlIsopropanol in1000mlIn a volumetric flask, dilute with double distilled water to the mark and shake well to obtain the internal standard solution. Take tetrahydrofuran and ethyl acetate separately0.1ml, Yu100mlDilute the volumetric flask with internal standard solution to the mark as the reference solution, and take0.4/Adetermination.

2.2 Preparation of sample solution: precise weighing1.50gSample in10mlAdd internal standard solution to the volumetric flask and dilute to the mark. Take0.1μLSample injection.

3 result

3.1 Determination of linear range of standard curve: take1.0mlIsopropanol in1000mlDilute with water to the mark in a volumetric flask, shake well, and use as the internal standard solution. Take ethyl acetate and tetrahydrofuran separately0.0005ml，0.005ml，0.01ml，0.02ml，0.04ml，0.06ml、0.08ml、0.10ml、0.12ml、0.16ml、0.18 a surnameml100mlDilute the volumetric flask with internal standard solution to the mark, shake well, and take0.4μLdetermination. Linear regression is performed with the concentration of the analyte on the x-axis and the ratio of the peak area of the analyte to the peak area of the internal standard on the y-axis,Tetrahydrofuran standard curve:y=1366.9x r=0.9996Ethyl acetate standard curve:y=981.9x r=0.9998

3.2 Determination of precision: Preparation of solution: Take1.0mlIsopropanol in1000mlAdd water to the mark in a volumetric flask and shake well to obtain the internal standard solution. Take tetrahydrofuran and ethyl acetate separately0.1ml、0.05ml、0.005mla surname100mlDilute to the mark with internal standard solution in a volumetric flask, and prepare for each concentration5A parallel sample, take0.4μLMeasure and calculate the relative standard deviation based on the area ratio of tetrahydrofuran, ethyl acetate, and isopropanol.

3.3 Determination of Recovery Rate: Take1.0mlIsopropanol in1000mlDilute the volumetric flask with water to the mark and shake well to obtain the internal standard solution. Take tetrahydrofuran separately（A）Ethyl acetate（B）every0.05ml、0.005mla surname100mlDilute the internal standard solution to the mark in a volumetric flask, shake well, and prepare each sample5Share, spare. Inject the sample and record the peak area. Calculate the recovery rate.

3.4 Detection limit and quantification limit: The detection limit of tetrahydrofuran is:1.778μg/mlThe quantitative limit is:3.556μg/mlThe detection limit for ethyl acetate is:1.804μg/mlThe quantitative limit is:3.608μg/ml.

4 discuss

4.1 This method uses internal standard method for quantitative calculation of production samples, which is very easy to operate and has high recovery rate and precision. After calculation, the separation degrees of tetrahydrofuran and isopropanol were determined to be4.95and2.83The symmetry factor is0.97and0.99Meeting and being suitable for analyzing residual solvents in drugs is beneficial for controlling drug quality.

4.2 In production, fast and timely completion of laboratory sampling and analysis work is the * requirement for product quality control. This method has been applied in the actual work of our factory, providing not only a true and accurate basis for production, but also a convenient and efficient method that has been reported by customers and confirmed to be qualified and accurate in product inspection. Worth promoting vigorously.