柱前衍生化气相色谱法测定莪术油中莪术醇含量___

目的：建立柱前衍生化气相色谱法测定莪术油中莪术醇含量。方法：采用N,O-双（三甲基硅氧烷）三氟乙酰胺-三甲基氯硅烷（99∶1）为柱前衍生化试剂，该试剂与莪术醇分子中的羟基定量发生反应，掩盖活性集团，衍生物产物易于分离及检测，并应用GC-MS进行了结构确证。以外标法测定了莪术油中莪术醇的含量。结果：莪术醇在0.05～1.02 mg•mL-1的范围内呈现出良好的线性关系，平均回收率（n=9）为99.5%。结论：该法准确、可靠，可用于莪术油的质量控制。
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Objective:A precolumn derivatization GC method was established to determine curcumol in Oleum Curcumae.Methods:By using BSTFA ，one reactive hydrogen of curcumol was substituted with siloxane.Then hydroxy of curcumol can be masked and polarity of curcumol can be lowered，so better peak shape and higher sensitivity can be got on middle or low polar capillary column.And derivatives can be confirmed by GC-MS.Results:The calibration curve of curcumol was in good linearity over the ranges of 0.05-1.02 mg•mL-1,and the average recovery(n=9) was 99.5%.Conclusion:The method is accurate，reliable and reproducible，and it can be adopted for the quality control of Oleum Curcumae.