第 42 卷第 6 期Vol. 42 No. 6
2012 年 12 月Dec 2012

所属栏目:分析与测试

顶空毛细管气相色谱法测定交联透明质酸钠凝胶中的残留溶剂
陈 涛1,薛明玲1,宋国强2,于培培2 (1. 常州药物研究所有限公司,江苏 常州 213000;2. 常州大学 制药与生命科学学院,江苏 常州 213164)
摘 要:采用顶空毛细管气相色谱法测定交联透明质酸钠凝胶中的残留溶剂。采用SE-30毛细管柱(50 m×0.53 mm×3.0 μm),FID检测器,检测器温度为250℃,进样口温度为180℃;柱温为50℃,保持2 min,以10℃/min的升温速率升到160℃,保持5 min;顶空进样,平衡温度为80℃,平衡时间为30 min,分流比为1∶1;溶剂为水。被测物均能得到很好的分离,峰面积与质量浓度线性关系良好,精密度和回收率良好。该方法可用于交联透明质酸钠凝胶中残留溶剂的测定。
关键词:毛细管气相色谱;交联透明质酸钠凝胶;残留溶剂
中图分类号:O657.7+1  文献标识码:A  文章编号:1009-9212(2012)06-0067-03
Determination of Residual Solvents in Cross-linked Sodium Hyaluronate Gel by CGC
CHEN Tao1,XUE Ming-ling1,SONG Guo-qiang2,YU Pei-pei2 (1. Changzhou Institute of Material Medical Co.,Ltd.,Changzhou 213000;2. College of Pharmacy & Life Science,Changzhou University,Changzhou 213164,China)
Abstract:To establish a method for the determination of residual solvents in cross-linked sodium hyaluronate gel with head-space capillary gas chromatography(CGC),a SE-30 capillary column(50 m×0.53 mm×3.0 μm)and hydrogen flame ionization detector(FID)were applied. The detector temperature was 250℃ and the injector temperature was 180℃. The column temperature was maintained at 50℃ for 2 min,then raised at a rate of 10℃/ min to 160℃ and maintained for 5 min. The sample was dissolved in water. The containers of head-space injector were in equilibrium at 80℃ for 30 min,and the splitting-ratio was 1∶1. The measured solvents were separated completely. The calibration curve of each solvent showed a good linear relationship with good precision and accuracy.
Key words:capillary gas chromatography;cross-linked sodium hyaluronate gel;residual solvents
基金项目:江苏省产学研前瞻性联合研究项目(BY2009122)。
作者简介:宋国强(1969-),男,江苏常州人,高级工程师,博士,主要从事药物中间体及电子化学品的合成与应用研究。(E-mail:drugs@vip.sina.com
联 系 人:于培培,硕士研究生,主要从事精细化工中间体的合成。(E-mail:yupeipei06435215@126.com)
收稿日期: 2012-12-1