It can be used for the detection of residual organic solvents in dichloromethane and 12-dichloroethane in cefazolin hydrochloride. 3.2 The method established in this paper is accurate and reliable. It is very important for the quality control and safe use of this product.
OBJECTIVE: To establish a method for the determination of residual organic solvents in dichloromethane and 12-dichloroethane in cefazolin hydrochloride. Methods Headspace Gas Chromatography. Results The analytes were well separated. Cefozopran Hydrochlorid fourth-generation cephalosporin antibiotics showed a good linear relationship between peak area and concentration, and the precision was good. Conclusion This method can be used for cefozopran hydrochloride hydrochloride drug substance. Detection of residual amounts of methylene chloride and 12-dichloroethane.
It shows broad-spectrum antibacterial activity against Gram-positive bacteria, Gram-negative bacteria and anaerobic bacteria. Compared with the third-generation cephalosporins, it enhances the activity against Gram-positive bacteria, especially for Streptococcus pneumoniae. It is also effective against Streptococcus faecalis, which is not sensitive to general cephalosporins, and has strong activity against C. faecalis and Enterobacter cloacae. Since a kind of solvent 12-dichloroethane and a second-class solvent methylene chloride were used in the synthesis of the drug, in order to control the product quality, the determination method of the above two residual solvents was established by GC headspace chromatography. .
1 instruments and reagents
Agilent 6890 gas chromatograph ; the reagents used were analytically pure except that 12-dichloroethane was chromatographically pure; the cefazolin hydrochloride bulk drug was provided by Yangzijiang Pharmaceutical Group Co., Ltd. (batch number)
2 test methods and results
Adhere to 10min headspace injection: headspace equilibrium temperature is 80 °C, 2.1 chromatographic conditions column: DB-5 capillary column (30m530μm 5μm column temperature: use sequential heating first at 80 ° C for 8 min and then at 30 ° C / min to 240 °C. Equilibration time is 30 min inlet temperature 180 ° C; detector: electron capture detector (ECD temperature 250 ° C; split ratio 11 carrier gas: high purity N2 flow rate 3.0 ml / min solvent: NN-dimethylformamide ( DMF
Precisely weighed, 2.2 special properties test to take the appropriate amount of dichloromethane, 12-dichloroethane. A mixed solution of 0.25 μg of 0.03 mg of 12-dichloroethane per 1 ml of dichloromethane was prepared by dilution with DMF as a reference solution. 1 ml of the blank solvent DMF and the reference solution were respectively placed in a headspace bottle, and the cells were injected under the above chromatographic conditions, and localized with a single standard solution of each solvent. The results indicate that a small amount of impurities in the DMF does not interfere with the analysis of the residual solvent.
The injection was repeated 6 times under the above chromatographic conditions. In the 2.3 precision test, 1 ml of the reference solution under the specific test item was placed in the headspace bottle. Record the chromatogram. The RSD of the peak area of ​​the analyte was 1.7% of dichloromethane and 5.0% of dichloroethane, respectively, indicating that the two solvents had good injection precision.
Precision weighed, 2.4 linear test to take the appropriate amount of dichloromethane, 12-dichloroethane. Separate the bottles separately, dilute with DMF to make a series of linear solutions, take 1ml of linear solution in the headspace bottle, inject under the above chromatographic conditions, record the chromatogram, and the peak area (A is the ordinate, to the concentration Cμg/ml was linearly regressed on the abscissa. The results indicated that the linear relationship of methylene chloride in the range of 25.9651.92 μg/ml 12-dichloroethane in the range of 0.19810.3962 μg/ml was good.
In a 10 ml volumetric flask, 2.5 samples were taken and 0.5 g of this product was accurately weighed. Dissolve in DMF and dilute to the mark as the test solution; the reference solution is prepared according to the method in 2.2. Take 1 ml of the reference solution and the test solution, respectively, in a headspace bottle, and inject under the above chromatographic conditions, and record the chromatogram. According to the external standard method, the peak area is calculated. The results are shown in Table 1, Table 1, three batches of samples, dichloromethane, 12-dichloroethane residue detection
3 discussion and summary
The HP-1HP-5 capillary column was used successively, and 3.1 chromatographic conditions were selected during the detection process. None of the good separation results were achieved, and the DB-5 capillary column was used, and the residual solvent and the blank solvent were completely separated.
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