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A novel fast method for aqueous derivatization of THC,OH‐THC and THC‐COOH in human whole blood and urine samples for routine forensic analyses 下载免费PDF全文
《Biomedical chromatography : BMC》2018,32(4)
A novel aqueous in situ derivatization procedure with propyl chloroformate (PCF) for the simultaneous, quantitative analysis of Δ9‐tetrahydrocannabinol (THC), 11‐hydroxy‐Δ9‐tetrahydrocannabinol (OH‐THC) and 11‐nor‐Δ9‐tetrahydrocannabinol‐carboxylic acid (THC‐COOH) in human blood and urine is proposed. Unlike current methods based on the silylating agent [N,O‐bis(trimethylsilyl)trifluoroacetamide] added in an anhydrous environment, this new proposed method allows the addition of the derivatizing agent (propyl chloroformate, PCF) directly to the deproteinized blood and recovery of the derivatives by liquid–liquid extraction. This novel method can be also used for hydrolyzed urine samples. It is faster than the traditional method involving a derivatization with trimethyloxonium tetrafluoroborate. The analytes are separated, detected and quantified by gas chromatography–mass spectrometry in selected ion monitoring mode (SIM). The method was validated in terms of selectivity, capacity of identification, limits of detection (LOD) and quantification (LOQ), carryover, linearity, intra‐assay precision, inter‐assay precision and accuracy. The LOD and LOQ in hydrolyzed urine were 0.5 and 1.3 ng/mL for THC and 1.2 and 2.6 ng/mL for THC‐COOH, respectively. In blood, the LOD and LOQ were 0.2 and 0.5 ng/mL for THC, 0.2 and 0.6 ng/mL for OH‐THC, and 0.9 and 2.4 ng/mL for THC‐COOH, respectively. This method was applied to 35 urine samples and 50 blood samples resulting to be equivalent to the previously used ones with the advantage of a simpler method and faster sample processing time. We believe that this method will be a more convenient option for the routine analysis of cannabinoids in toxicological and forensic laboratories. 相似文献
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Michael A. Schafroth Giuseppe Zuccarello Simon Krautwald Dr. David Sarlah Prof. Dr. Erick M. Carreira 《Angewandte Chemie (International ed. in English)》2014,53(50):13898-13901
All four stereoisomers of Δ9‐tetrahydrocannabinol (Δ9‐THC) were synthesized in concise fashion using stereodivergent dual catalysis. Thus, following identical synthetic sequences and applying identical reaction conditions to the same set of starting materials, selective access to the four stereoisomers of THC was achieved in five steps. 相似文献
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毛细管气相色谱法对大麻中主要成分的定性定量分析 总被引:6,自引:0,他引:6
采用毛细管气相色谱法测定大麻中大麻酚、四氢大麻酚和大麻二酚的含量。以氯仿为提取溶剂,甲醇为色谱溶剂,用HP-5(10m×0.53mm×2.65μm)柱,以柱温220℃进行测定。大麻二酚、四氢大麻酚和大麻酚在20~120mg/L的浓度范围内线性关系良好,r分别为0.9994,0.9991和0.9995,回收率分别为97.3%~104.0%,97.3%~106.6%和95.3%~102.4%,最低检测限均为0.2μg/mL。利用3种主要成分保留时间的良好重现性也可进行定性。方法简便、快速、准确、灵敏。 相似文献
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Hamid Asiabi Yadollah Yamini Maryam Shamsayei Tahmine Baheri 《Journal of separation science》2020,43(6):1128-1136
A novel plate‐like nano‐sorbent based on copper/cobalt/chromium layered double hydroxide was synthesized by a simple coprecipitation method. The synthesized nanoparticels were introduced into a stainless steel cartridge using a dry packing method. Then, the packed cartridge was introduced as a novel on‐line “packed in‐tube” configuration and followed by high performance liquid chromatography for the determination of trace amounts of ?9‐tetrahydrocannabinol from biological samples and cannabis leaves. The as‐prepared sorbent exhibited long lifetime, good chemical stability, and high anion‐exchange capacity. Several important factors affecting the extraction efficiency, such as extraction and desorption times, pH of the sample solution and flow rates of the sample and eluent solutions, were investigated and optimized. Under optimized conditions, this method showed good linearity for ?9‐tetrahydrocannabinol in the ranges of 0.09–500, 0.3–500, and 0.4–500 µg/L with coefficients of determination of 0.9999, 0.9991, and 0.9994 in water, serum and plasma samples, respectively. The inter‐ and intra‐assay precisions (n = 3) were respectively in the ranges of 1.8–4.6% and 1.9–4.0% at three concentration levels of 10, 50, and 100 µg/L. The limits of detection were also in the range of 0.02–0.1 µg/L. 相似文献
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建立了大麻毒品中主要有效成分Δ9-四氢大麻酚的液相色谱分析方法.选择甲醇作为大麻植物或大麻树脂的提取溶剂.采用岛津ODS-SP型(150 mm×4.6 mm,5μm)色谱柱作为定量方法的标准柱,紫外检测器主定量波长为210 nm,辅定量波长为195 nm或220 nm.以水-乙腈为流动相进行梯度洗脱,流速1mL/min,柱温40℃,进样量10 μL.在优化条件下,△9-四氢大麻酚在0.5~ 100.0 mg/L范围内线性良好,外标法及内标法的相关系数(r2)均大于0.99999.方法的检出限(S/N≥3.3)和定量下限(S/N≥ 10)分别为0.12 mg/L和0.40 mg/L.用该方法检测某大麻树脂样本,△9-四氢大麻酚含量的不确定度评定结果为5.32%±0.17%,k=2.实验结果表明,该方法快速、灵敏、准确、可靠,适用于大麻植物及树脂的定量测定. 相似文献
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《Analytical letters》2012,45(1):7-11
Abstract Quantitative gas chromatography of small amounts of δ1 - tetrahydrocannabinol has been demonstrated on a variety of silicone columns. Retention data in the form of methylene unit values were obtained on these columns. 相似文献
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Iwamuro Y Iio-Ishimaru R Chinaka S Takayama N Hayakawa K 《Biomedical chromatography : BMC》2012,26(11):1452-1456
Δ9‐Tetrahydrocannabinol is the primary psychoactive component in cannabis, one of the most commonly used illicit drugs in the world. This paper describes a simple and rapid method for direct analysis of major metabolites of Δ9‐tetrahydrocannabinol; 11‐nor‐Δ9‐tetrahydrocannabinol‐9‐carboxylic acid and its glucuronide in urine by capillary electrophoresis/mass spectrometry. The only pretreatment needed for a urine sample was dilution with methanol containing an internal standard and centrifugation. Electrophoresis was carried out in an untreated fused‐silica capillary (50 µm i.d. × 85 cm) filled with 40 m m ammonium formate (pH 6.4). An analysis could be completed within 10 min. For both compounds, the assay was linear over the range 0.1 ? 10 µg/mL in urine with correlation coefficients (r2) > 0.99 and the limit of detection was 0.5 pg (10 nL injection). The detection yields and reproducibilities were determined at three different concentrations (0.1, 0.5 and 2 µg/mL in urine). The mean detection yields were 60 ? 99%. The intra‐ and inter‐day relative standard deviations of migration times were 0.063 ? 0.19 and 0.18 ? 0.36%, and those of peak areas were 4.2 ? 18 and 5.9 ? 25%, respectively. The proposed method successfully analyzed the urine samples of cannabis users. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
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Delta9-tetrahydrocannabinolic acid A (Delta9-THCA-A) is the precursor of Delta9-tetrahydrocannabinol (Delta9-THC) in hemp plants. During smoking, the non-psychoactive Delta9-THCA-A is converted to Delta9-THC, the main psychoactive component of marihuana and hashish. Although the decarboxylation of Delta9-THCA-A to Delta9-THC was assumed to be complete--which means that no Delta9-THCA-A should be detectable in urine and blood serum of cannabis consumers--we found Delta9-THCA-A in the urine and blood serum samples collected from police controls of drivers suspected for driving under the influence of drugs (DUID). For LC-MS/MS analysis, urine and blood serum samples were prepared by solid-phase extraction. Analysis was performed with a phenylhexyl column using gradient elution with acetonitrile. For detection of Delta9-THCA-A, the mass spectrometer (MS) (SCIEX API 365 triple-quadrupole MS with TurboIonSpray source) was operated in the multiple reaction monitoring (MRM) mode using the following transitions: m/z357 --> 313, m/z357 --> 245 and m/z357 --> 191. Delta9-THCA-A could be detected in the urine and blood serum samples of several cannabis consumers in concentrations of up to 10.8 ng/ml in urine and 14.8 ng/ml in serum. The concentration of Delta9-THCA-A was below the Delta9-THC concentration in most serum samples, resulting in molar ratios of Delta9-THCA-A/Delta9-THC of approximately 5.0-18.6%. Only in one case, where a short elapsed time between the last intake and blood sampling is assumed, the molar ratio was 18.6% in the serum. This indicates differences in elimination kinetics, which need to be investigated in detail. 相似文献
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