Abstract: Objective: To establish a convenient and rapid method for the determination of the residual solvents ethyl acetate and tetrahydrofuran in the raw material powder of cefotaxime sodium. Method: Shimadzu GC-17A gas chromatograph, nitrogen gas as carrier gas, isopropanol as internal standard, and temperature-programmed measurement. Results: The precision of this method for measuring ethyl acetate and tetrahydrofuran were (0.70 ~ 1.87) and (1.34 ~
1.91). The method recoveries were 100.2 ± 2.7 and 101.1 ± 3.6, respectively. Conclusion: This method is suitable for the determination of residual solvent of cefotaxime sodium, and the method is simple and fast.
Keywords: cefotaxime sodium; residual solvent; gas chromatography
Determ ination of the COncentratiOn of Residual Solvent in Cefotaxim e Sodium Raw Powder by GC M ethod
Li Chengjun, et a1. Harbin Pharmaceutical Factory (150086)
Abstract: Objective: T0 build a GC—method for determining the concentration of trithy lamine and tetrahydrofuran in cefotaxime raw powder. M ethod: the samples were determined by SHIM UZU GC-1 17A heated by computerized control with isopropyl aleohol as the internal standard. Result: the assay precision of method to determine acetoactic ester and tetrahydrofuran were (0.70 to 1.87) and (1.34 to 1.91). 'the recovery rate of it were 100.2 ± 2.7 and 101.1 ± 3.6. Conclusion: the method was convenient and fast for detecting the resdual in eefotaxime.
Key words: cefotaxime sodium; residual solvent; GC-method
Cefotaxime sodium is the third-generation broad-spectrum cephalosporin antibiotic, which is widely used in clinic. Its quality directly affects the clinical efficacy. Therefore, rapid and accurate detection of product quality is an effective means to ensure high-quality products. In the process of testing the quality of cefotaxime sodium produced by our factory in accordance with the standards of the Pharmacopoeia, we tried to establish a new, simple and accurate gas chromatography method for the determination of residual solvents in cefotaxime sodium synthesis The method can quickly and effectively detect the residual solvent, and it is a method worth promoting.
1 Experimental part
1.1 Experimental instrument: GC-17A gas chromatograph: FID detector; chromatographic column: HP-FFAP (cross-linked polyethylene glycol-TPA, 25em × 0.25mm × 0.25μm (film thickness).
1.2 Reagents: ethyl acetate, tetrahydrofuran, and isopropanol are chromatographically pure (Shanghai Chemical Reagent Research Institute), all water used in the experiment is double distilled water (chromatographic test without interference peaks).
1.3 Chromatographic conditions: nitrogen gas as carrier gas, column pressure 100Kpa, split ratio 200: 1, detector temperature 250 ℃, inlet temperature 200 ℃. The initial temperature of the column temperature (programmed temperature increase) is 55 ° C, which is retained for 1.7 minutes, and then it is raised to 90 ° C at a rate of 30 ° C / min, and retained for 1 minute.
2 Sample determination
2.1 Preparation of internal standard solution and reference solution: Take 1.0ml of isopropanol in a 1000ml volumetric flask, add double distilled water to dilute to the mark and shake well as the internal standard solution. Take 0.1ml each of tetrahydrofuran and ethyl acetate, respectively, in a 100ml volumetric flask and dilute to the mark with the internal standard solution, as a reference solution, take 0.4 / A for determination.
2.2 Preparation of sample solution: Weigh 1.50g of sample in a 10ml volumetric flask, add internal standard solution to dilute to the mark, and take 0.1μL of sample.
3 results
3.1 Determination of the linear range of the standard curve: Take 1.0ml of isopropanol in a 1000ml volumetric flask, dilute with water to the mark, shake well as the internal standard solution. Separately take ethyl acetate, tetrahydrofuran 0.0005ml, 0.005ml, 0.01ml, 0.02ml, 0.04ml,
0.06ml, 0.08ml, 0.10ml, 0.12ml, 0.16ml, 0.18 add internal standard solution to ml100ml volumetric flask and dilute to the mark, shake well, and take 0.4μL for determination. Taking the concentration of the substance to be measured as the abscissa, the area formed by the baseline of the substance to be measured is called the peak area. A = × σ × h = 2.507σh = 1.064 Wh / 2h> The ratio of the peak area to the peak area of ​​the internal standard is linear regression on the ordinate, tetrahydrofuran standard curve: y = 1366.9x r = 0.9996
Standard curve of ethyl acetate: y = 981.9x r = 0.9998
3.2 Determination of precision: Preparation of the solution: Take 1.0 ml of isopropanol in a 1000 ml volumetric flask, add water to the mark and shake well as the internal standard solution. Take 0.1ml, 0.05ml and 0.005ml of tetrahydrofuran and ethyl acetate respectively in 100ml volumetric flasks, dilute to the mark with internal standard solution, prepare 5 parallel samples of each concentration, take 0.4μL and measure with tetrahydrofuran Calculate the relative standard deviation of the area ratio of ethyl acetate to isopropanol.
3.3 Determination of recovery rate: Take 1.0ml of isopropanol in a 1000ml volumetric flask and dilute with water to the mark and shake well as the internal standard solution. Take 0.05ml and 0.005ml of tetrahydrofuran (A) and ethyl acetate (B) respectively in 100ml volumetric flask, add internal standard solution to dilute to the mark, shake well, prepare 5 samples for each sample, and set aside. Inject and record the peak area. Calculate the recovery rate.
3.4 Detection limit and quantification limit: The detection limit of tetrahydrofuran is: 1.778μg / ml, and the limit of quantification is: 3.556μg / ml. The detection limit of ethyl acetate is: 1.804 μg / ml, and the limit of quantification is: 3.608 μg / ml.
4 Discussion
4.1 This method uses the internal standard method to quantify the production samples, the operation is very simple, and the recovery rate and precision are convenient. The calculated resolutions of tetrahydrofuran and isopropanol were 4.95 and 2.83, and the symmetry factors were 0.97 and 0.99. It meets and is suitable for the detection requirements of analyzing residual solvents in medicines, which is conducive to the quality control of medicines.
4.2 In the production, it is the first requirement of product quality control to quickly and timely do the analysis and analysis of laboratory samples. This method is
This article comes from the determination of residual solvent content in cefotaxime sodium by gas chromatography | Scientific Instrument Online Original Link: http: //
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