顶空气相色谱法同时测定药品包装复合膜中9种残留溶剂  

Simultaneous determination of nine kinds of residual organic solvents in laminated films used for drug packages by head-space gas chromatography

作　　者：张亚红[1] 米亚娴[1] 

机构地区：[1]天津市药品检验所,天津300070

出　　处：《天津药学》2013年第5期15-17,共3页Tianjin Pharmacy

摘　　要：目的:建立一种用于测定药品包装复合膜中常见的9种残留溶剂含量的顶空气相色谱方法。方法:选用TR-WAX(30 mm×0.53 mm,1.0μm)毛细管色谱柱,载气(氮气)流速为2.0 ml/min,采用程序升温:初始温度为50℃(保持0 min),以20℃/min的速率升温至70℃(保持4 min),再以40℃/min的速率升温至160℃(保持14 min),FID检测器温度为230℃,进样口温度为230℃。结果:9种有机溶剂在20 min内能很好的分离,9种残留溶剂线性关系良好,相关系数均大于0.998,加标回收率在90.8%～98.3%,相对标准偏差RSD(n=6)在2.63%～6.13%,检出限范围为0.004～0.008 mg/m2。结论:该法快速、准确、灵敏度高,适用于药品包装复合膜中溶剂残留量的同时测定。Objective ： An analytical method was developed for the determination of 9 kinds of residual organic solvents in laminated films used for drug packages by head -space gas chromatography. Methods：The optimal chromatographic conditions are as follows ： a TR - WAX capillary column （ 30 mm × 0.53 mm, 1.0 μm ） , nitrogen as carrier gas with a flow rate of 2.0 ml/min, column temperature programmed from 50℃ （ hold 0 min ） to 70 ℃ at a rate of 20 ℃/min and kept at 70 ℃ for 4 min, and then from 70℃ to 160℃ at a rate of 40 ℃/min and kept at 160℃ for 14 min; flame ionization detector temperature 230℃ and injector temperature 230 ℃. Resuhs ： All the 9 kinds of organic residues were separated well within 20 min, the standard curves were linear （ r 〉 0.998） ,the recoveries were 90.8% - 98.3% with RSD （ n = 6） in the range of 2.63% - 6.13% , and the limits of detection （S/N = 3 ）were 0. 004 -0. 008 mg/m2. Conclusion：This method is rapid, convenient, sensitive and can be used for the determination of residual organic solvents in laminated films used for drug packages.

关 键 词：顶空 气相色谱 有机溶剂 残留 药品包装复合膜 

分 类 号：R927.11[医药卫生—药学]