GC法测定4,7-二氯喹啉中的有关物质

Determination of impurities in 4,7-dichloroquinoline by GC

目的建立一种快速、准确测定4,7-二氯喹啉中的杂质乙氧基次甲基丙二酸二乙酯(EMME)、4,5-二氯喹啉和4,8-二氯喹啉的气相色谱法。方法采用Elite-1701毛细管色谱柱(30 m×0.53 mm×0.5μm),柱温为初始温度180℃恒温4 min,以6.5℃/min升至200℃恒温0 min,再以20℃/min升至250℃恒温4 min,进样口温度为300℃,进样量为1μL,分流比为10∶1,FID检测器温度为280℃。结果 EMME、4,5-二氯喹啉和4,8-二氯喹啉分别在2.601~7.803、2.501~7.503、2.531~7.593μg/mL质量浓度范围内与色谱峰面积呈良好线性关系(r>0.999);平均回收率分别为101.50%(RSD=2.90%)、97.55%(RSD=2.86%)、101.31%(RSD=2.81%)。结论建立的方法简便、准确,适用于4,7-二氯喹啉中EMME、4,5-二氯喹啉和4,8-二氯喹啉的测定。

Objective To establish a rapid and sensitive gas chromatography method for the determination of diethyl ethoxymethylene malonate(EMME),4,5-dichloroquinoline and 4,8-dichloroquinoline in 4,7-dichloroquinoline.Methods The chromatographic column was elite-1701(30 m×0.53 mm×0.5 μm).The column temperature was programmed to be 180℃ for 4 min,and then was raised at a rate of 6.5 ℃/min to 200 ℃ and held for 0 min,and was finally raised at a rate of 20 ℃/min to 250 ℃ and held for 4 min.The injection port temperature was 300 ℃,the injection volume was 1 μL,the split ratio was 10:1,and the temperature of FID detector was 280 ℃.Results EMME,4,5-dichloroquinoline and 4,8-dichloroquinoline showed good linear relationships in the concentration range2.601-7.803 μg/mL,2.501-7.503 μg/mL,2.531-7.593 μg/mL(r>0.999).The recoveries of the three impurities were 101.50%(RSD=2.90%),97.55%(RSD=2.86%),101.31%(RSD=2.81%).Conclusion The method is simple and accurate,which is suitable for the determination of EMME,4,5-dichloroquinoline and 4,8-dichloroquinoline in4,7-dichloroquinoline.