基于核磁共振技术的川芎多指标质量评价研究

Multi-index quality evaluation of Chuanxiong Rhizoma based on NMR

目的:采用氢核磁定量方法快速测定川芎中主要成分阿魏酸、藁本内酯、洋川芎内酯A的含量。方法:以氘代二甲基亚砜为测试溶剂,吡嗪为内标物,在600 MHz光谱仪上进行1H-qNMR测量,其中吡嗪、阿魏酸、藁本内酯、洋川芎内酯A的定量共振峰分别为δ8.66、δ6.35~6.37、δ5.53~5.55、δ5.93~5.96。结果:阿魏酸、藁本内酯、洋川芎内酯A的线性关系良好,相关系数分别为0.9999、0.9999、0.9991,精密度RSD分别为1.4%、0.34%、0.83%,回收率分别为96.1%~103.9%(RSD=3.0%)、97.0%~103.5%(RSD=3.0%)和97.0%~102.3%(RSD=2.4%),表明所建立的氢核磁定量方法,结果准确,稳定可行,且整个检测过程在3 min左右完成。3批川芎药材中阿魏酸、藁本内酯、洋川芎内酯A的含量范围分别为1.508~1.612、10.887~11.503、8.349~9.051 mg·g^(-1)。结论:该方法操作简单,分析速度快、专属性强,可用于川芎中3个有效成分的同步测定,为川芎药材的全面质量评价和质量控制提供科学依据。

Objective:To establish a hydrogen nuclear magnetic quantitative method which can rapidly determine the contents of ferulic acid,ligustilide and senkyunolide A in Chuanxiong Rhizoma.Methods:Using dimethyl sulfoxide-d6(DMSO-d6)as the test solvent and pyrazine as the internal standard,1 H-qNMR measurement was performed on a 600 MHz spectrometer.The quantitative resonance peaks of pyrazine,ferulic acid,ligustilide,and senkyunolide A wereδ8.66,δ6.35-6.37,δ5.53-5.55 andδ5.93-5.96,respectively.Results:The linear relationship,limit of detection and limit of quantitation,precision,stability,and recovery were verified and the results were good.The linear correlation coefficients of ferulic acid,ligustilide and senkyunolide A were good with r of 0.9999,0.9999 and 0.9991,respectively.The RSDs of precision were 1.4%,0.34%and 0.83%,and the recoveries were 96.1%-103.9%(RSD=3.0%),97.0%-103.5%(RSD=3.0%)and 97.0%-102.3%(RSD=2.4%),respectively,which indicated that the established method was accurate,stable and feasible.And the whole detection process was completed in about three minutes.The contents of three components in three batches of Chuanxiong Rhizoma were 1.508-1.612 mg·g^(-1)(ferulic acid),10.887-11.503 mg·g^(-1)(ligustilide)and 8.349-9.051 mg·g^(-1)(senkyunolide A).Conclusion:The 1H-qNMR method has the advantages of simple operation,fast analysis speed and strong specificity,and can be used for the simultaneous determination of 3 active components in Chuanxiong Rhizoma,providing a scientific basis for the overall quality evaluation and quality control of Chuanxiong Rhizoma.