Department of Marine Living Resources, Iranian National Institute for Oceanography, Tehran, Iran.
J Chromatogr B Analyt Technol Biomed Life Sci. 2011 Oct 1;879(27):2897-901. doi: 10.1016/j.jchromb.2011.08.020. Epub 2011 Aug 22.
A headspace solid-phase microextraction (HS-SPME) coupled to gas chromatography-mass spectrometry (GC-MS) method was developed to determine a type of terpenoid named as cantharidin in the false blister beetles, family Oedemeridae. The experimental parameters for HS-SPME method were optimized. Six commercial fibers for HS-SPME method development were tested and the divinylbenzene/carboxene/polydimethylsiloxane fiber was selected to provide the best detection of analyzed compound. The calibration curve showed linearity in the range of 0.1-50 μg mL(-1), correlation coefficient (R(2)=0.992), limit of detection (0.01 ng mL(-1)) and quantitation (0.04 ng mL(-1)) were obtained for the proposed method. The relative standard deviations of intra-day and inter-day assays were 7.8 and 3.4%, respectively. The recovery values, obtained after spiking the beetle samples by three concentration levels of standard solution, were higher than 87%. The results indicated the successful application of the proposed method on the analysis of cantharidin from the false blister beetles.
建立了一种顶空固相微萃取（HS-SPME）与气相色谱-质谱联用（GC-MS）的方法，用于检测芫菁科假芫菁体内的一种萜烯类化合物斑蝥素。对 HS-SPME 方法的实验参数进行了优化。对 6 种商品化的 HS-SPME 萃取纤维进行了测试，结果表明二乙烯基苯/羧基/聚二甲基硅氧烷纤维对分析物的检测效果最佳。所提出的方法在 0.1-50 μg mL(-1) 的范围内呈现出良好的线性关系，相关系数（R(2)=0.992）、检测限（0.01 ng mL(-1))和定量限（0.04 ng mL(-1))均令人满意。日内和日间测定的相对标准偏差分别为 7.8%和 3.4%。通过在甲虫样品中加入 3 个浓度水平的标准溶液进行加标回收实验，回收率均高于 87%。这些结果表明，所提出的方法可成功应用于假芫菁体内斑蝥素的分析。
