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首页> 外文学位 >Determination of psilocybin and psilocin in hallucinogenic mushrooms by HPLC with diode array and MS detection.
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Determination of psilocybin and psilocin in hallucinogenic mushrooms by HPLC with diode array and MS detection.

机译：高效液相色谱-二极管阵列和质谱检测法测定致幻蘑菇中的香菇菌素和香菇素。

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摘要

Psilocin and psilocybin are the main active components in hallucinogenic mushrooms. However, their chromatographic quantification has been problematic due in part to the poor chromatographic separation of these compounds, co-elution of interfering compounds, and incomplete extraction of psilocin and psilocybin from mushroom samples. Therefore, a study was undertaken to optimize (1) the extraction of these compounds from mushrooms and (2) the quantification of psilocin and psilocybin by reversed phase high performance liquid chromatography (RP-HPLC) with diode array or mass spectrometry (MS) detection. The effects of the mobile phase on the presence of interfering compounds, the relative separation, and peak shape were examined for psilocybin, psilocin, bufotenine and tryptamine (internal standard). Factors examined included, buffer concentration, buffer type, buffer pH and organic phase type. These parameters all affected chromatographic separations, with the largest effect seen when the buffer type or pH were changed. A short and effective extraction procedure was also developed to quantify these analytes by RP-HPLC with diode array detection and to qualitatively identify them by RP-HPLC with mass spectrometry detection. The estimated detection limit of this method, with a signal-to-noise ratio of three, was 10 ng/mL for diode array detection and 0.1 ng/mL for MS detection of psilocin and psilocybin in methanolic mushroom extracts. Psilocin and psilocybin were stable for a minimum of one year when stored in an acidic methanolic solution that was sparged with high purity nitrogen gas, sealed in an amber vial and stored at -11°C.;Keywords. Forensic Science, psilocybin, psilocin, reverse phase high performance liquid chromatography, liquid chromatography mass spectrometry, hallucinogenic mushrooms, HPLC
机译：幽菌素和梭菌霉素是致幻蘑菇中的主要活性成分。但是，它们的色谱定量存在问题，部分原因是这些化合物的色谱分离差，干扰化合物的共洗脱以及蘑菇样品中loclocin和psilocybin的提取不完全。因此，进行了一项研究，以优化（1）从蘑菇中提取这些化合物，以及（2）通过带有二极管阵列或质谱（MS）检测的反相高效液相色谱（RP-HPLC）对psilocin和psilocybin进行定量。检查了倍半新霉素，倍半新霉素，丁苯丁烯酸和色胺（内标）的流动相对干扰化合物的存在，相对分离和峰形的影响。检查的因素包括缓冲液浓度，缓冲液类型，缓冲液pH和有机相类型。这些参数均影响色谱分离，改变缓冲液类型或pH值时效果最大。还开发了一种短而有效的提取程序，通过带有二极管阵列检测的RP-HPLC对这些分析物进行定量，并通过带有质谱检测的RP-HPLC对这些分析物进行定性鉴定。该方法的估计检出限（信噪比为3）对于二极管阵列检测为10 ng / mL，对于MS检出甲醇蘑菇提取物中的loclocin和psilocybin为MS的0.1 ng / mL。硅氧菌素和psilocybin在储存于酸性甲醇溶液中稳定至少一年，该酸性溶液中充满高纯度氮气，密封在琥珀色小瓶中并在-11°C下保存。法医科学，psilocybin，psilocin，反相高效液相色谱，液相色谱质谱，致幻蘑菇，HPLC

著录项

  • 作者

    Van Orden, Raymond C.;

  • 作者单位

    State University of New York College of Environmental Science and Forestry.;

  • 授予单位 State University of New York College of Environmental Science and Forestry.;
  • 学科 Anthropology Medical and Forensic.;Chemistry Biochemistry.
  • 学位 M.S.
  • 年度 2008
  • 页码 111 p.
  • 总页数 111
  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类
  • 关键词

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