摘要
目的:建立气相色谱法(GC)测定羟苯甲、乙、丙、丁酯中的甲醇、乙醇、正丙醇、异丙醇、正丁醇、异丁醇、仲丁醇和叔丁醇8种有机溶剂残留量。方法:采用DB-624毛细管柱(0.32 mm×30 m,1.8μm);FID检测器;进样口温度为200℃,检测器温度为250℃;载气为高纯氮气,载气流速为2 mL·min^-1;柱温为升温程序,起始温度45℃,保持2 min,以5℃·min^-1升温至65℃保持5 min,再以40℃·min^-1升温至200℃保持3 min。结果:8种残留溶剂在各自浓度范围内线性关系良好(r均>0.999);羟苯甲、乙、丙、丁酯的平均回收率在102.1%~106.0%。结论:本法操作简单、准确度高、重现性好,可用于羟苯甲酯、乙酯、丙酯、丁酯中8种有机溶剂残留量的测定。
Objective:To establish a GC method for simultaneous determination of the eight residual solvents of methanol,ethanol,n-propanol,isopropanol,n-butanol,isobutanol,sec-butanol and tert-butanol in methy paraben,ethyl paraben,propyl paraben and buthyl paraben.Methods:The determination was performed on DB-624 capillary column(0.32 mm×30 m,1.8μm)under the programmed temperature.FID was used,the inlet temperature was 200℃and the detector temperature was 250℃.The high pure nitrogen was as the carrier gas and the flow rate of carrier gas was 2 mL·min^-1.The column temperature programme was set as:remain the starting temperature of 45℃for 2 min,increase to 65℃at the rate of 5℃·min^-1 and remain 65℃for 5 min,then increase to 200℃at the rate of 40℃·min^-1 and remain 200℃for 3 min.Results:The eight residual solvents had a good linear relationship in the respective concentration ranges(r>0.999).The average recovery rates were 102.1%-106.0%.Conclusion:The established method is simple,accurate and reproducible.It can be used for the determination of 8 organic solvents residues in methy paraben,ethyl paraben,propylparaben and buthylparaben.
作者
谢莹莹
刘雁鸣
龙海燕
李颖
XIE Yingying;LIU Yanming;LONG Haiyan;LI Ying(Hunan Institute for Drug Control(Hunan Pharmaceutical Excipients Testing and Inspection Center);Hunan Engineering&Technology Research Center for Pharmaceutical Quality Evaluation,Changsha 410001,China)
出处
《中国药品标准》
CAS
2020年第3期249-253,共5页
Drug Standards of China
关键词
残留溶剂
GC法
羟苯甲酯
羟苯乙酯
羟苯丙酯
羟苯丁酯
residual solvents
GC method
methy paraben
ethyl paraben
propyl paraben
buthyl paraben
