摘要
建立了用毛细管气相色谱法测定芳樟醇合成工艺路线中过程样品组分含量的方法。采用HP FFAP(30m×0 32mmi d ×0 25μm)毛细管柱,以氢火焰离子化检测器检测,N2为载气,流速0 6mL/min,分流比150∶1,并采用程序升温,以校正面积归一化法计算各组分的含量。在确定的色谱条件下,样品中各组分分离较好,分析周期仅18min。含量在50%以上的1 氯代异戊烯、甲基庚烯酮、芳樟醇、去氢芳樟醇等主要组分含量测定的相对标准偏差小于0 5%,回收率为99 7%～100 9%。结合标样、气相色谱 质谱(GC/MS)和气相色谱 红外光谱(GC/FTIR)对样品中各组分进行了定性,组分的MS和FTIR定性结果与图谱库匹配在90%以上,定性结果正确可靠。方法可以用于芳樟醇合成工艺中过程样品及芳樟醇成品的分析。
Samples from linalool synthesis were determined using area normal ization method by capillary gas chromatography with FID detection and an HP-FFA P capillary column (30 m×032 mm id×025 μm) under programmed temperatu re. The carrier gas was nitrogen, the flow-rate was 06 mL/min, and the sp ilt ratio was 150∶1. With this method, the samples were well separated and the analysis time was only 18 minutes. RSDs for compounds of 1-choloro-3-methyl- 2-butene, 6-methyl-5-hepten-2-one, linalool and dehydrolinalool, were less than 05%, and the recoveries were 997%-1009%. The contents of these compo unds were more than 50%. In comparison with standard samples and using GC/MS and GC/FTIR methods, the compounds of samples were identified, and the matches were more than 90%. The results of identification were reliable. The method is suita ble for the analys is of samples from the synthesis process of linalool and its products.
出处
《色谱》
CAS
CSCD
北大核心
2003年第4期424-426,共3页
Chinese Journal of Chromatography
