摘要
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％二甲基聚硅氧烷的AT-1石英毛细管柱，载气为氮气，流速为1．0mL·min^-1。检测器温度为250℃；进样口温度为200℃；程序升温为初始温度40℃，保持8min，以10℃·min^-1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0．9970和0．9997；平均回收率95．0％～103．8％，精密度均小于2．0％，最低检出限分别为0．48μg·mL^-1和0．09μg·mL^-1。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。
To establish a method of head-space capillary gas chromatography for the determination of residual solvents in polyvinyl alcohol. The residual solvents in polyvinyl alcohol were separated by AT-1 capillary column with an FID detector. The carried gas was nitrogen. The injector temperature and the detector temperature were controlled at 200℃ and 250℃, respectively. The programmed column temperature was set as follows, maintained at 40℃ for 8 min and then raised to 150℃ at the rate of 10℃·min^-1 followed by holding for 2min. The sample dissolved in water and acetone was used as the internal standard. The containers of head-space injector were in equilibrium at 80℃ for 30min, the splittingratio was 1 ： 1. The detected solvents were separated completely. The calibration curve of each solvent showed a good linear relationship （r： 0. 9970 and 0. 9997） with good precision and accuracy （not more than 2. 0%）. The average recovery rate was in the range of 95.0%-103.8%. The LOD of methanol and methyl acetate was 0. 48μg·mL^-1 and 0.09μg·mL^-1. The established method was accurate and reliable. It can be used for the determination of residual solvents in polyvinyl alcohol.
出处
《中国药事》
CAS
2008年第6期474-476,共3页
Chinese Pharmaceutical Affairs
关键词
聚乙烯醇
残留溶剂
顶空气相色谱法
polyvinyl alcohol
residual solvent
headspace gas chromatography
