气相色谱法测定2,6-二氯苯酚的杂质  

Determination of impurity in 2, 6-dichlorophenol by gas chromatography

作　　者：王金虎 鲜婧 张云 WANG Jin-hu;XIAN Jing;ZHANG Yun(Shandong Key Lab of Chemical Drugs,Shandong Academy of Pharmaceutical Sciences,Jinan 250101)

机构地区：[1]山东省药学科学院山东省化学药物重点实验室,济南250101

出　　处：《中南药学》2018年第9期1272-1274,共3页Central South Pharmacy

摘　　要：目的建立2,6-二氯苯酚中已知杂质邻氯苯酚和对氯苯酚的含量测定方法。方法采用气相色谱法(GC),色谱柱为Agilent DB-624气相色谱毛细管柱(30 m×0.32 mm,1.8μm),载气为高纯氮气,检测器为氢火焰离子化检测器(FID),进样口及检测器温度分别为220℃和280℃,柱温采用程序升温。结果各已知杂质峰与相邻峰间均能良好的分离;邻氯苯酚的定量限为12.08 ng,检测限为3.62ng;对氯苯酚的定量限为20.52 ng,检测限为6.16 ng;邻氯苯酚与对氯苯酚在10~300μg·mL^(-1)与峰面积有良好的线性关系;平均回收率分别在99.5%~104.8%,97.9%~101.6%,RSD均小于1%。结论该方法操作简单,结果可靠准确,可用于2,6-二氯苯酚中杂质的测定。Objective To establish a method for the determination of known impurities o-chlorophenol and p-chlorophenol in 2, 6-dichlorophenol. Methods Gas chromatography （GC） and Agilent DB-624 gas chromatography capillary column （30 m × 0.32 mm, 1.8 μm） were used. The carrier gas was high purity nitrogen, and the detector was hydrogen flame ionization detector （FID）. The temperature of inlet and detector was 220 ℃ and 280 ℃ respectively, and the column temperature increased with the program. Results Various known impurity peaks and adjacent peaks were well separated. The limit of quantification for o-chlorophenol was 12.08 ng and the detection limit was 3.62 ng. The limit of quantification for p-chlorophenol was 20.52 ng, with detection limit 6.16 ng. There was a good linearity for o-chlorophenol and p-chlorophenol at 10-300 μg · mL - 1. The average recoveries were at 99.5%-104.8% and 97.9%-101.6%, respectively, and the RSD was less than 1%. Conclusion The method is simple, reliable and accurate, and can be used for the determination of impurities in 2, 6-dichlorophenol.

关 键 词：2 6-二氯苯酚 邻氯苯酚 对氯苯酚 气相色谱法 

分 类 号：R927[医药卫生—药学]