Zhou Jun, Sun Xiao Li, Wang Si Wang
Department of chemistry, Fourth Military Medical University, Xi'an, Shanxi 710032, China.
J Chromatogr A. 2008 Jul 25;1200(2):93-9. doi: 10.1016/j.chroma.2008.04.070. Epub 2008 May 3.
A new method based on micelle-mediated extraction and cloud-point preconcentration was developed for the separation and determination of hydrophobic compounds osthole and imperatorin from Cnidium monnieri by high performance liquid chromatography with photodiode array detection. The non-ionic surfactant C(13)E(8) (Genapol X-080) was chosen as the extract solvent. Various experimental conditions were investigated to evaluate and optimize the extraction and preconcentration process. The chromatographic separation was accomplished on a Zorbax SB-C(18) analytical column (150 mm x 4.6mm i.d., 5 microm particle diameter) maintained at 30 degrees C and detected by UV absorption at 320 nm. The gradient elution was achieved with a mobile phase composed of 0.1% phosphoric acid and acetonitrile at a flow rate of 1.0 mL min(-1). Under the optimum conditions, the calibration curve for both analytes was linear in the range of 0.52-33.5 microg mL(-1) with the correlation coefficients greater than 0.9996. The intra-day and inter-day precision (RSD) is below 5.3% and the limits of detection (LOD) for the analytes are 93 and 124 ng mL(-1)(S/N=3). The proposed technique is a low cost, simple and sensitive method with high clean-up effect. Finally, the method was successfully applied to separate and determine osthole and imperatorin from C. monnieri, respectively.
建立了一种基于胶束介导萃取和浊点预富集的新方法，用于通过高效液相色谱-光电二极管阵列检测从蛇床子中分离和测定疏水性化合物蛇床子素和欧前胡素。选择非离子表面活性剂C(13)E(8)（Genapol X-080）作为萃取溶剂。研究了各种实验条件以评估和优化萃取和预富集过程。色谱分离在Zorbax SB-C(18)分析柱（150 mm×4.6mm内径，5μm粒径）上进行，柱温保持在30℃，通过320nm处的紫外吸收进行检测。流动相由0.1%磷酸和乙腈组成，以1.0 mL min(-1)的流速进行梯度洗脱。在最佳条件下，两种分析物的校准曲线在0.52-33.5μg mL(-1)范围内呈线性，相关系数大于0.9996。日内和日间精密度（RSD）低于5.3%，分析物的检测限（LOD）分别为93和124 ng mL(-1)（S/N=3）。所提出的技术是一种低成本、简单且灵敏的方法，具有高净化效果。最后，该方法成功应用于分别从蛇床子中分离和测定蛇床子素和欧前胡素。
