顶空气相色谱法测定聚乙烯醇中甲醇和乙酸甲酯的残留量 - 中国药事.pdfVIP

474 2008 22 6 药品检验 药品质量 孙会敏, 赵 霞, 王 颖 ( , 100050) : 建立顶空气相色谱法测定聚乙烯醇有机溶剂残留量采用气相色谱法测定, 固定相为100% 甲 1 基聚硅氧烷的AT1 石英毛细管柱, 载气为氮气, 流速为10mL min 检测器温度为250 ; 进样口温 1 度为200 ; 程序升温为初始温度40 , 保持8min, 以 10 min 升温至150 , 保持 2min顶空进 样, 平衡温度为 80 , 平衡时间为30min, 分流比为1 ! 1, 水为溶剂, 丙酮为内标物被测物甲醇乙 酸甲酯和内标丙酮在此色谱条件下均能得到很好的分离, 空白对照无干扰, 峰面积与检测浓度呈良好的线 性关系, 相关系数r 分别为09970 和09997; 平均回收率950%~ 1038%, 精密度均小于20%, 最低 1 1 检出限分别为048 mL 和009 mL 本试验建立的色谱方法灵敏准确, 适合药用辅料聚乙烯 醇原料中有机溶剂残留量的检测 : 聚乙烯醇; 残留溶剂; 顶空气相色谱法 : R917 : A : ( 2008) Determination of Residual Solvents inPolyvinyl Alcohol by Headspace GC Sun Huimin, Zhao Xia and Wan Yin ( National Institute for the Control of Pharmaceutical and Biolo ical Products, Beijin 100050) ABSTRACT T o establish a method of head- space capillary as chromato raphy for the determination of residual solvents in polyvinyl alcohol. T he r esidual solvents in polyvinyl alcohol w ere separated by AT - 1 capillary column w ith an FID detector. T he carried as w as nitro en. The injector temperature and the detector temperatur e w ere controlled at 200 and 250 , respectively. T he pro r ammed column temperature w as set as follow s: maintained at 40 for 8 min and then raised to 150 at the rate of 10 1 min follow ed by holdin for 2min. T he sample dissolved in w ater and acetone w as used as the internal standard. The containers of head- space injector w ere in equilibr ium at 80 for 30min, the splittin - ratio was 1 ! 1. The detected solvents w ere separ ated completely . T he calibration curve of each solvent show ed a ood linear relationship ( r : 09970 and 09997) w ith ood pr eci