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目的:建立顶空毛细管气相色谱法测定盐酸克林霉素中有机溶剂残留量。方法:采用顶空气相色谱法,色谱柱为DB-624毛细管柱,载气为氮气,流速为2 ml·min-1,分流比为1∶1。FID检测器,检测器温度为300℃;进样口温度为200℃;柱温采取程序升温,起始温度40℃,保持5 min,以20℃·min-1升温至200℃,持续10 min。顶空进样,平衡温度为80℃,平衡时间为30 min。以水为溶剂,外标法测定盐酸克林霉素中甲醇,乙醇,丙酮,三氯甲烷和N,N-二甲基甲酰胺的残留量。结果:在此色谱条件下,各有机溶剂均能得到有效分离,在所考察的浓度范围内线性关系良好,r=0.9991~0.9999;平均回收率为97.2%~101.2%,RSD为0.68%~1.98%(n=9)。结论:本试验建立的顶空气相色谱方法适合盐酸克林霉素原料中有机溶剂残留量的检测。
Objective: To establish a method for the determination of residual organic solvents in clindamycin hydrochloride by headspace capillary gas chromatography. Methods: Headspace gas chromatography was used. The column was DB-624 capillary column. The carrier gas was nitrogen and the flow rate was 2 ml · min-1. The split ratio was 1: 1. FID detector, detector temperature was 300 ℃; inlet temperature was 200 ℃; column temperature was programmed temperature, the initial temperature was 40 ℃, maintained for 5 min, the temperature was raised to 200 ℃ at 20 ℃ · min-1 for 10 min . Headspace injection, the equilibrium temperature is 80 ℃, the balance time is 30 min. Water as solvent, external standard method for determination of clindamycin hydrochloride methanol, ethanol, acetone, chloroform and N, N-dimethylformamide residues. Results: Under these chromatographic conditions, each organic solvent could be effectively separated. The linear range was 0.9991 ~ 0.9999, the average recovery was 97.2% ~ 101.2% and the RSD was 0.68% ~ 1.98 % (n = 9). Conclusion: The headspace gas chromatography method established in this study is suitable for the determination of residual organic solvents in clindamycin hydrochloride raw materials.