首页> 外文期刊>Analytical and bioanalytical chemistry >Molecularly imprinted polymer for selective determination of Δ~9-tetrahydrocannabinol and 11-nor-Δ~9-tetrahydrocannabinol carboxylic acid using LC-MS/MS in urine and oral fluid
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Molecularly imprinted polymer for selective determination of Δ~9-tetrahydrocannabinol and 11-nor-Δ~9-tetrahydrocannabinol carboxylic acid using LC-MS/MS in urine and oral fluid

机译:分子印迹聚合物,用于通过尿液和口腔液中的LC-MS / MS选择性测定Δ〜9-四氢大麻酚和11-nor-Δ〜9-四氢大麻酚羧酸

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The use of molecularly imprinted polymers (MIPs) for solid phase extraction (MISPE) allows a rapid and selective extraction compared with traditional methods. Determination of Δ~9-tetrahydrocannabinol (THC) and 11- nor-Δ~9-tetrahydrocannabinol carboxylic acid (THC-COOH) in oral fluid (OF) and urine was performed using homemade MISPEs for sample clean-up and liquid chromatography tandem mass spectrometry (LC-MS/MS). Cylindrical MISPE shaped pills were synthesized using catechin as a mimic template. MISPEs were added to 0.5 mL OF or urine sample and sonicated 30 min for adsorption of analytes. For desorption, the MISPE was transfered to a clean tube, and sonicated for 15 min with 2 mL acetone:acetonitrile (3:1, v/v). The elution solvent was evaporated and reconstituted in mobile phase. Chromatographic separation was performed using a SunFire C18 (2.5 μm; 2.1×20 mm) column, and formic acid 0.1%and acetonitrile asmobile phase, with a total run time of 5 min. The method was fully validated including selectivity (no endogenous or exogenous interferences), linearity (1– 500 ng/mL in OF, and 2.5–500 ng/mL in urine), limit of detection (0.75 and 1 ng/mL in OF and urine, respectively), imprecision (%CV <12.3 %), accuracy (98.2–107.0 % of target), extraction recovery (15.9–53.5 %), process efficiency (10.1–46.2 %), and matrix effect (
机译:与传统方法相比,将分子印迹聚合物(MIP)用于固相萃取(MISPE)可以实现快速,选择性的萃取。使用自制的MISPE进行样品净化和液相色谱串联质谱分析,测定口服液(OF)和尿液中的Δ〜9-四氢大麻酚(THC)和11-或Δ〜9-四氢大麻酚羧酸(THC-COOH)光谱法(LC-MS / MS)。使用儿茶素作为模拟模板合成圆柱形MISPE形状的药丸。将MISPEs加入0.5 mL OF或尿液样品中,超声处理30分钟以吸附分析物。为了解吸,将MISPE转移到干净的试管中,并用2 mL丙酮:乙腈(3:1,v / v)超声处理15分钟。蒸发洗脱溶剂,并在流动相中重构。使用SunFire C18(2.5μm; 2.1×20 mm)色谱柱,使用0.1%的甲酸和乙腈作为流动相进行色谱分离,总运行时间为5分钟。该方法已得到充分验证,包括选择性(无内源性或外源性干扰),线性度(OF中为1-500 ng / mL,尿液中为2.5-500 ng / mL),检出限(OF和0.75中和1 ng / mL尿液),不精确度(%CV <12.3%),准确度(目标的98.2-107.0%),提取回收率(15.9-53.5%),加工效率(10.1-46.2%)和基质效应(<?55% )。分析物在自动进样器中稳定72小时。在OF中可以确保以1:10的比例稀释,Quantisal?基质效应显示出离子抑制作用(<?80.4%)。该方法用于20 OF和11尿样的分析。这是使用MISPE技术测定OF中THC和THC-COOH的第一种方法。

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