浮小麦5-二十一烷基间苯二酚提取与测定方法优化及指纹图谱研究

Study on the Optimization of Extraction and Determination Method and Fingerprint of Triticum aestivum L.

目的:建立浮小麦5-二十一烷基间苯二酚含量的HPLC法测定及指纹图谱研究的方法。方法:采用正交试验法对提取工艺进行优化,采用戴安Ultimate 3000全自动高效液相色谱仪对色谱条进行优化,用HPLC法对浮小麦5-二十一烷基间苯二酚含量进行测定及指纹图谱研究,用“中药色谱指纹图谱相似度评价系统”(2004A)进行相似度分析,用SPSS 22.0分析软件对指纹图谱进行聚类分析。结果:优化提取工艺为甲醇超声30 min提取1次;优化色谱条件分别是“1.3.2.1”、“1.3.3.1”项下色谱条件;14批浮小麦中5-二十一烷基间苯二酚含量在1.62~5.02 mg·g^-1之间,平均加样回收率为101.16%,RSD为0.7%。浮小麦HPLC指纹图谱有18个共有峰,其中保留时间(Rt)为60.780 min对应的峰是5-二十一烷基间苯二酚,与共有模式相比较,S11相似度为0.988,其余样品相似度均达到0.99以上。结论:建立的浮小麦5-二十一烷基间苯二酚的含量测定和浮小麦药材HPLC指纹图谱的方法稳定可靠,可用于浮小麦5-二十一烷基间苯二酚含量测定和鉴别,为浮小麦的质量控制和评价奠定基础。

Objective:To establish a HPLC method for the determination of 5-heneicosyresorcinol in aestivum and study on its fingerprint.Methods:Orthogonal test was used to optimize the extraction process,dai'an ultimate 3000 automatic high performance liquid chromatograph was used to optimize the chromatographic strip,HPLC was used to determine the content of 5-heneicosyresorcinol inaestivum and the fingerprint was studied.Similarity analysis was carried out with“similarity evaluation system of chromatographic fingerprint of traditional Chinese medicine”(2004A),and cluster analysis was carried out with SPSS 22.0 analysis software.Results:The optimized extraction process was methanol extraction for 30 min,the optimized chromatographic conditions were“1.3.2.1”and“1.3.3.1”and the content of 5-heneicosyresorcinol in 14 batches of aestivum ranged from 1.62 mg·g^-1 to 5.02 mg·g^-1,with an average recovery of 101.16%and RSD of 0.7%.There are 18 common peaks in the HPLC fingerprint of aestivum,among which the retention time(RT)is 60.780 min and the corresponding peak is 5-heneicosyresorcinol.Compared with the common pattern,the similarity of S11 is 0.988,and the similarity of other samples is above 0.99.Conclusion:The established method for the determination of 5-heneicosyresorcinol in aestivum and HPLC fingerprint of aestivum is stable and reliable.It can be used for the determination and identification of 5-heneicosyresorcinol in aestivum and lay a foundation for the quality control and evaluation of aestivum.