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液相色谱-紫外检测法与气相色谱-电子捕获检测法联用测定尿液中Δ⁹-四氢大麻酚-11-酸。

Combination of liquid chromatography with ultraviolet detection and gas chromatography with electron-capture detection for the determination of delta 9-tetrahydrocannabinol-11-oic acid in urine.

作者信息

Karlsson L, Roos C

出版信息

J Chromatogr. 1984 Mar 9;306:183-9. doi: 10.1016/s0378-4347(00)80881-6.

Abstract

A method is described for the determination of delta 9-tetrahydrocannabinol-11-oic acid (delta 9-THC-11-oic acid) in urine by using a combination of liquid chromatography and glass capillary gas chromatography with electron-capture detection. Prior to extraction, the glucuronide conjugate of delta 9-THC-11-oic acid was enzymatically converted to the free acid and delta 8-THC-11-oic acid added as an internal standard. An aliquot of the extract was separated by liquid chromatography and one eluate fraction containing delta 8-THC-11-oic and delta 9-THC-11-oic acids was collected. Before gas chromatographic analysis the acids were converted to their pentafluoropropyl-pentafluoropropionyl derivatives. Authentic urine samples, positive with the EMIT cannabinoid assay, were analysed and the results compared with those obtained from an earlier described gas chromatographic-mass spectrometric method. The detection limit for the overall method was approximately 20 ng/ml. The precision was 8% for a sample concentration of 90 ng/ml of delta 9-THC-11-oic acid in urine.

摘要

本文描述了一种采用液相色谱与玻璃毛细管气相色谱联用并结合电子捕获检测法来测定尿液中δ9 - 四氢大麻酚 - 11 - 酸(δ9 - THC - 11 - 酸)的方法。在提取之前,δ9 - THC - 11 - 酸的葡萄糖醛酸共轭物经酶促转化为游离酸,并加入δ8 - THC - 11 - 酸作为内标。取一部分提取物通过液相色谱进行分离,收集一个含有δ8 - THC - 11 - 酸和δ9 - THC - 11 - 酸的洗脱液馏分。在进行气相色谱分析之前,将这些酸转化为它们的五氟丙基 - 五氟丙酰衍生物。对经EMIT大麻素检测呈阳性的真实尿液样本进行分析,并将结果与先前描述的气相色谱 - 质谱法所获得的结果进行比较。该整体方法的检测限约为20 ng/ml。对于尿液中δ9 - THC - 11 - 酸浓度为90 ng/ml的样本,精密度为8%。

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