莪术醇的分离鉴定及含量测定

An isolation Identification and Quantification of Curcumol

目的:研究从莪术油中提取莪术醇的方法,建立莪术醇含量分析的新方法。方法:以莪术油为原料,进行减压蒸馏,收集208～216℃的馏分经重结晶得到产品,将其和对照品作差示量热光谱、红外光谱、核磁共振和质谱对比分析确定莪术醇;用高效液相色谱法测定其含量,色谱柱为ODS柱;以乙腈∶水(15∶85,V∶V)为流动相;流速为1.0mL/min;检测波长为210nm;柱温为25℃;以外标两点法计算含量。结果:经差示扫描量热光谱、红外光谱、核磁共振、质谱分析鉴定提取的产物是莪术醇,高效液相分析其浓度在10～70μg/mL范围内线性关系良好,相关系数r=0.9999(n=7);精密度试验RSD为0.92%(n=6);平均回收率为99.86%,RSD=0.76%,含量为98.9%,RSD=0.89%(n=3)。日内日间差异实验RSD均小于0.78%,表明样品稳定性良好。结论:减压蒸馏法提取莪术醇的工艺流程简单,适合大规模生产,而且纯度高;高效液相色谱法测定莪术醇含量的方法简便、准确、快速,可用于莪术醇及其制剂的质量控制。

Objective ：To investigate a method of isolation of curcumol form Zedoary turmeric oil, and to establish a new method to quantify the content of cureumol. Method ：Zedoary turmeric oil was applied for reduced pressure distillation ,and the fraction of distillate at 208 -216℃ was assembled, recrysted in order to get the product. The products were identified by DSC, IR, NMR and MS in comparison with the curcumol control. The content of curcumol was determined by HPLC. The sample was separated on Diamonsll C18 （5μm ,200mm × 4.6mm）column with the mobile phase of acetoni- trile - water （ 15 ： 85 ,volume ratio）. The detection was performed at 210nm, the flow rate was 1.0mL/min and the temperature of the column is 25℃. The contents of curcumol were calculated by external standard method. Results ：The product is identified as curcumol by DSC ,IR, NMR and MS spectra;the calibration curve was linear in the range of 10 - 70μg/mL and the correlation coefficient was 0. 9999 ;The RSD was 0.92% （ n = 7）in the precision test ;The average recovery rate and RSD were 99.86% and 0.76% （ n =6） ,respectively. The contents of cureumol extracted from curcuma oll and RSD were 98.9% and 0.89% （ n = 3 ）, respectively. The RSD of inter - day and intra - day was under 0.78% that indicated the samples were stable. Conclusion ：The method used here to isolate curcumol form Zedoary turmeric oil is simple, suitable applied for large - scale production with high purity; the described HPLC method to determine the content of curcumol is simple ,accurate and rapid. It may be applied for quality control in the routine analysis of curcumol and its preparation.