顶空毛细管气相色谱法测定羟戊基苯甲酸钾中的残留溶剂  

Determination of residual solvent in potassium-hydroxypentyl benzoate by headspace capillary GC

作　　者：张艳红 吕昭云 张颖 张秋佳 张宝军 

机构地区：[1]国家新药开发工程技术研究中心北京科莱博医药开发有限责任公司,北京102600 [2]北京协和药厂,北京102600

出　　处：《药物分析杂志》2009年第9期1565-1567,共3页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立顶空毛细管气相色谱法测定羟戊基苯甲酸钾中的残留溶剂。方法:采用气相色谱法测定,以0.1mol·L-1氢氧化钠溶液为溶解介质,甲醇为内标;色谱柱为石英毛细管柱(DB-1,60m×0.32mm×1μm),FID检测器,载气为氮气。结果:二氯甲烷、丙酮、乙醇均能得到有效分离;线性范围分别为1.7～170,10～1000,10～1000μg·mL-1(r=0.9991～0.9998);平均回收率为98.0%～103.7%。结论:本方法灵敏,准确可靠,可用于羟戊基苯甲酸钾原料药中有机溶剂残留量的检测。Objective： To establish a method of headspace capillary GC for the determination of residual solvents in potassium - hydroxypentyl benzoate. Methods： The residual solvents （ dichloromethane, acetone, ethanol） were sepa- rated by DB - 1 capillary column（60 m ×0. 32 mm × 1 μm） with an FID detector. The carried gas was nitrogen. The sample was dissolved in 0. 1 mol ·L-1 caustic soda solution, methanol was used as the internal standard. Re- suits： Three residual solvents （ dichloromethane, acetone, ethanol） were completely separated ; The calibration curves were linear in the ranges of 1.7 - 170,10 - 1000,10 - 1000 μg · mL - 1 （ r = 0. 9991 - 0. 9998 ）, respectively ; The average recovery was in the range of 98.0% -103.7%. Conclusion ：The established method is accurate and relia- ble, and can be used for the determination of residual solvents in potassium - hydroxypentyl benzoate.

关 键 词：顶空毛细管气相色谱法 羟戊基苯甲酸钾 残留溶剂 

分 类 号：R917[医药卫生—药物分析学]