LC-MS/MS analysis of Δ9-tetrahydrocannabinolic acid A in serum after protein precipitation using an in-house synthesized deuterated internal standard.
LC-MS/MS analysis of Δ9-tetrahydrocannabinolic acid A in serum after protein precipitation using an in-house synthesized deuterated internal standard.
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使用内部合成的氘代内标对蛋白质沉淀后血清中的 α9-四氢大麻酸 A 进行 LC-MS/MS 分析
DOI：
10.1002/jms.3021
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发表时间：
2012
期刊：
影响因子：
--
通讯作者：
Auwärter V
中科院分区：
文献类型：
--
作者：
Wohlfarth A;Roth N;Auwärter V
提出了一种基于液相色谱/串联质谱法的测定方法，用于快速、精确和灵敏地定量血清中的 Δ9-四氢大麻酸 A (THCA)。 THCA 是大麻中 Δ9-四氢大麻酚的生物前体，引起了药理学和法医学领域的兴趣，特别是作为最近大麻使用的潜在标记物。添加由 D3-THC 合成的氘化 THCA 作为起始材料和蛋白质沉淀后，在 Luna C18 柱（150 × 2.0 mm × 5 μm）上使用浓度为 0.1% 的梯度洗脱分离分析物。甲酸和乙腈/0.1%甲酸。数据采集是在三重四极杆线性离子阱质谱仪上以负电喷雾电离的多反应监测模式进行的。优化后，使用以下样品制备程序：向 200 μL 血清中加入内标溶液和甲醇，然后用 500 μL 冰冷的乙腈“分批”沉淀。储存和离心后，蒸发上清液，并将残留物重新溶解在流动相中。该检测方法根据国际指南进行了全面验证，包括首次评估基质效应和稳定性实验。检测限为 0.1 ng/mL，定量限为 1.0 ng/mL。该方法被发现具有选择性，并证明使用 1/x 加权校准模型在 1.0 至 100 ng/mL 范围内呈线性，回归系数 >0.9996。准确度和精密度数据均在规定范围内（RSD ≤ 8.6%，偏差：2.4%~11.4%），提取率大于84%。经过3次冻融循环并在-20°C保存1个月后，血清样品中的分析物稳定。版权所有 © 2012 约翰·威利父子有限公司
An assay based on liquid chromatography/tandem mass spectrometry is presented for the fast, precise and sensitive quantitation of Δ9‐tetrahydrocannabinolic acid A (THCA) in serum. THCA is the biogenetic precursor of Δ9‐tetrahydrocannabinol in cannabis and has aroused interest in the pharmacological and forensic field especially as a potential marker for recent cannabis use.After addition of deuterated THCA, synthesized from D3‐THC as starting material, and protein precipitation, the analytes were separated using gradient elution on a Luna C18 column (150 × 2.0 mm × 5 µm) with 0.1% formic acid and acetonitrile/0.1% formic acid. Data acquisition was performed on a triple quadrupole linear ion trap mass spectrometer in multiple reaction monitoring mode with negative electrospray ionization. After optimization, the following sample preparation procedure was used: 200 μL serum was spiked with internal standard solution and methanol and then precipitated ‘in fractions’ with 500 μL ice‐cold acetonitrile. After storage and centrifugation, the supernatant was evaporated and the residue redissolved in mobile phase.The assay was fully validated according to international guidelines including, for the first time, the assessment of matrix effects and stability experiments. Limit of detection was 0.1 ng/mL, and limit of quantification was 1.0 ng/mL. The method was found to be selective and proved to be linear over a range of 1.0 to 100 ng/mL using a 1/xweighted calibration model with regression coefficients >0.9996. Accuracy and precision data were within the required limits (RSD ≤ 8.6%, bias: 2.4 to 11.4%), extractive yield was greater than 84%. The analytes were stable in serum samples after three freeze/thaw cycles and storage at −20 °C for one month. Copyright © 2012 John Wiley & Sons, Ltd.
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未加热的大麻提取物及其主要化合物 THC-酸具有潜在的免疫调节特性，不受 CB1 和 CB2 受体偶联途径介导。
影响因子：
5.6
作者：
K. Verhoeckx;H. Korthout;A. P. van Meeteren;K. Ehlert;Mei Wang;J. van der Greef;R. Rodenburg;R. Witkamp
通讯作者：
R. Witkamp
影响因子：
2.3
作者：
Jung, Julia;Meyer, Markus R.;Auwaerter, Volker
通讯作者：
Auwaerter, Volker
影响因子：
2.3
作者：
Jung, Julia;Kempf, Juergen;Weinmann, Wolfgang
通讯作者：
Weinmann, Wolfgang
大麻中的植物大麻素 : : 生物合成酶的最新研究
DOI：
--
发表时间：
2007
期刊：
Chemistry and Biodiversity (In press)(印刷中)
影响因子：
--
作者：
Futoshi Taura;Supaart Sirikantaramas;Yukihiro Shoyama;Satoshi Morimoto
通讯作者：
Satoshi Morimoto
根据血浆 Δ9-四氢大麻酚和 11-正-9-羧基-Δ9-四氢大麻酚浓度估计最后一次使用大麻的时间
DOI：
--
发表时间：
2005
期刊：
影响因子：
--
作者：
M. Huestis;Allan J. Barnes;Michael L. Smith
通讯作者：
Michael L. Smith