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采用基质固相分散萃取-高效液相色谱-二极管阵列检测法分析拉帕烷型倍半萜内酯在川西獐牙菜根中的含量。

Matrix solid-phase dispersion extraction coupled with HPLC-diode array detection method for the analysis of sesquiterpene lactones in root of Saussurea lappa C.B.Clarke.

机构信息

Institute of Medicine and Drug Research, Qiqihar Medical University, Qiqihar 161006, China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2011 Sep 15;879(26):2809-14. doi: 10.1016/j.jchromb.2011.08.008. Epub 2011 Aug 17.

Abstract

We developed a reliable and effective method to determine costunolide and dehydrocostuslactone in the root of Saussurea lappa C. B.Clarke using matrix solid-phase dispersion (MSPD) extraction, HPLC separation and diode array detection (DAD). Several extraction parameters for the MSPD were optimized. Florisil was chosen as dispersing adsorbent with methanol as elution solvent. The ratio of Florisil to sample was selected to be 4:1 and no additional clean-up steps were needed. Linearities (r>0.9995) were determined to be in the range of 22.5-360.0 μg/mL for costunolide and 25.0-400.0 μg/mL for dehydrocostuslactone. Intra- and inter-day precisions were also determined with a relative standard deviation (RSD) less than 3.2%. The limits of detection were found to be 0.122 μg/mL for costunolide and 0.135 μg/mL for dehydrocostuslactone. The recoveries were in the range of 92.5-99.8% with relative standard deviations ranged from 1.2% to 3.5%. The proposed MSPD method required shorter time and lower solvent volume than maceration-ultrasonic and Soxhlet extraction methods.

摘要

我们开发了一种可靠有效的方法,使用基质固相分散(MSPD)萃取、HPLC 分离和二极管阵列检测(DAD)来测定川西獐牙菜根中的土木香内酯和去氢木香内酯。对 MSPD 的几个萃取参数进行了优化。弗罗里硅土被选为分散吸附剂,甲醇为洗脱溶剂。弗罗里硅土与样品的比例选择为 4:1,不需要额外的净化步骤。土木香内酯的线性范围为 22.5-360.0 μg/mL,去氢木香内酯的线性范围为 25.0-400.0 μg/mL,线性度(r>0.9995)。日内和日间精密度的相对标准偏差(RSD)均小于 3.2%。土木香内酯的检测限为 0.122 μg/mL,去氢木香内酯的检测限为 0.135 μg/mL。回收率在 92.5-99.8%之间,相对标准偏差在 1.2%-3.5%之间。与浸渍-超声提取和索氏提取方法相比,所提出的 MSPD 方法所需时间更短,溶剂体积更小。

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