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1.
A rapid, sensitive and selective determination of delta 9-tetrahydrocannabinol (THC) in human plasma, serum and saliva was developed with high-performance liquid chromatography with electrochemical detection. Initially, samples were deproteinized, followed by a one step liquid-liquid extraction. Samples were measured by high-performance liquid chromatography with electrochemical detection with 4-dodecylresorcinol as the internal standard. The minimal detectable limit for THC in biological samples was ca. 1 ng/ml with a signal-to-noise ratio greater than 3, corresponding to an on-column sensitivity for THC of ca. 0.5 ng. The detector was operated at + 0.90 V vs. Ag/AgCl and exhibited linearity over a concentration range of 1-150 ng/ml with correlation coefficients of the standard curves greater than 0.99.  相似文献   

2.
A two-dimensional (2D) gas chromatography/electron impact-mass spectrometry (GC/EI-MS) method for simultaneous quantification of Delta(9)-tetrahydrocannabinol (THC), 11-hydroxy-Delta(9)-tetrahydrocannabinol (11-OH-THC), and 11-nor-Delta(9)-tetrahydrocannabinol-9-carboxylic acid (THCCOOH) in human plasma was developed and validated. The method employs 2D capillary GC and cryofocusing for enhanced resolution and sensitivity. THC, 11-OH-THC, and THCCOOH were extracted by precipitation with acetonitrile followed by solid-phase extraction. GC separation of trimethylsilyl derivatives of analytes was accomplished with two capillary columns in series coupled via a pneumatic Deans switch system. Detection and quantification were accomplished with a bench-top single quadrupole mass spectrometer operated in electron impact-selected ion monitoring mode. Limits of quantification (LOQ) were 0.125, 0.25 and 0.125 ng/mL for THC, 11-OH-THC, and THCCOOH, respectively. Accuracy ranged from 86.0 to 113.0% for all analytes. Intra- and inter-assay precision, as percent relative standard deviation, was less than 14.1% for THC, 11-OH-THC, and THCCOOH. The method was successfully applied to quantification of THC and its 11-OH-THC and THCCOOH metabolites in plasma specimens following controlled administration of THC.  相似文献   

3.
A rapid and sensitive method for the simultaneous confirmatory analysis of three forensic most relevant cannabinoids, Delta(9)-tetrahydrocannabinol (THC), 11-hydroxy-Delta(9)-tetrahydrocannabinol (11-OH-THC) and 11-nor-9-carboxy-Delta(9)-tetrahydrocannabinol (THC-COOH), by means of high-performance liquid chromatography/tandem mass spectrometry (LC/MS/MS) in human plasma was developed and fully validated. Sample clean-up was performed by automated silica-based solid-phase extraction and the separation was carried out using a PhenylHexyl column (50 x 2 mm i.d., 3 micro m) and acetonitrile-5 mM ammonium acetate gradient elution. Data were acquired with an API 3000 LC/MS/MS system equipped with a turboionspray interface and triple quadrupole mass analyzer using positive electrospray ionization and multiple reaction monitoring. Two MS/MS transitions for each substance were monitored and deuterated analogues of analytes were used as internal standards for quantitation. The limit of quantitation was 0.8 ng ml(-1) for THC, 0.8 ng ml(-1) for 11-OH-THC and 4.3 ng ml(-1) for THC-COOH and linearity with a correlation coefficient r(2) = 0.999 was achieved up to 100 ng ml(-1) for THC and 11-OH-THC and 500 ng ml(-1) for THC-COOH. The limits of detection were 0.2 ng ml(-1) for THC, 0.2 ng ml(-1) for 11-OH-THC and 1.6 ng ml(-1) for THC-COOH. The developed LC/MS/MS method was also successfully used for the determination of THC-COOH-glucuronide, the phase II metabolite of THC-COOH.  相似文献   

4.
The detection and confirmation of cannabinoids in oral fluid are important in forensic toxicology. Currently, the presence of Δ9-tetrahydrocannabinol (THC) is used for the detection of cannabis in oral fluid. A low concentration of 11-nor-9-carboxy-Δ9-tetrahydrocannabinol (THC-COOH) is found in oral fluid, which suggested a convenient and low-sensitivity confirmation assay can be used in a routine forensic laboratory. In this study, a highly sensitive isotope dilution liquid chromatography–tandem mass spectrometry method following dansylation was successfully developed for simultaneous determination of THC and THC-COOH in oral fluid. The dansylated derivatives dramatically demonstrated and enhanced the sensitivity of THC and THC-COOH. To avoid signal influenced by the matrix, a 5-min liquid chromatography gradient program was evaluated and optimized, which reduced the sample diffusion and caused sharp peaks (less than 12 s) and thus helped to achieve detection at a low level. The sensitivity, accuracy, and precision were also evaluated, and high quantitative accuracy and precision were obtained. The limit of quantitation of this approach was 25 pg/mL for THC and 10 pg/mL for THC-COOH in oral fluid. Finally, the method was successfully applied to eight suspected cannabis users. Among them, in six oral fluid samples THC-COOH was determined at a concentration from 13.1 to 47.2 pg/mL.  相似文献   

5.
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,Obis(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   

6.
For the detection of the major active component of cannabis, Δ9-tetrahydrocannabinol (THC) in aqueous samples, a homogeneous competitive immunoassay based on fluorescence quenching induced by fluorescence resonance energy transfer (FRET) has been developed. The fluorescence of anti-THC-antibody, labeled with fluorescence dye DY-481XL, can be quenched after its binding to THC-BSA-quencher conjugate (bovine serum albumin coupled with THC and another fluorescence dye, DYQ-661, as quencher). This quenching effect is inhibited when the antibodies bind to free THC in aqueous sample, thus competing for binding sites with the THC-BSA-quencher conjugate. The extent of the inhibition corresponds to the concentration of THC in the samples. The assay principle is simple and the test duration is within 10 min. The detection limit for THC in buffer was 2 ng mL−1. In pooled saliva samples a detection limit of 50 ng mL−1 was achieved.  相似文献   

7.
Oral fluid (OF) is a valuable biological alternative for clinical and forensic drug testing. Evaluating OF to plasma (OF/P) cannabinoid ratios provides important pharmacokinetic data on the disposition of drug and factors influencing partition between matrices. Eleven chronic cannabis smokers resided on a closed research unit for 51 days. There were four 5-day sessions of 0, 30, 60, and 120 mg oral ?9-tetrahydrocannabinol (THC)/day followed by a five-puff smoked cannabis challenge on Day 5. Each session was separated by 9 days ad libitum cannabis smoking. OF and plasma specimens were analyzed for THC and metabolites. During ad libitum smoking, OF/P THC ratios were high (median, 6.1; range, 0.2–348.5) within 1 h after last smoking, decreasing to 0.1–20.7 (median, 2.1) by 13.0–17.1 h. OF/P THC ratios also decreased during 5-days oral THC dosing, and after the smoked cannabis challenge, median OF/P THC ratios decreased from 1.4 to 5.5 (0.04–245.6) at 0.25 h to 0.12 to 0.17 (0.04–5.1) at 10.5 h post-smoking. In other studies, longer exposure to more potent cannabis smoke and oromucosal cannabis spray was associated with increased OF/P THC peak ratios. Median OF/P 11-nor-9-carboxy-THC (THCCOOH) ratios were 0.3–2.5 (range, 0.1–14.7) ng/μg, much more consistent in various dosing conditions over time. OF/P THC, but not THCCOOH, ratios were significantly influenced by oral cavity contamination after smoking or oromucosal spray of cannabinoid products, followed by time-dependent decreases. Establishing relationships between OF and plasma cannabinoid concentrations is essential for making inferences of impairment or other clinical outcomes from OF concentrations.  相似文献   

8.
In the present study, an ultra-sensitive and highly reproducible novel SERS-based capillary platform was developed and utilized for the trace detection of tetrahydrocannabinol (THC). The approach combines the advantages of microwave-assisted nanoparticle synthesis, plasmonics and capillary forces. By employing a microwave-assisted preparation method, glass capillaries were reproducibly coated with silver nanoparticles in a batch fabrication process that required a processing time of 3 min without needing to use any pre-surface modifications or add surfactants. The coated capillaries exhibited an excellent SERS activity with a high reproducibility and enabled the detection of low concentrations of target molecules. At the same time, only a small amount of analyte and a short and simple incubation process was required. The developed platform was applied to the spectroscopic characterization of tetrahydrocannabinol (THC) and its identification at concentration levels down to 1 nM. Thus, a highly efficient detection system for practical applications, e.g., in drug monitoring/detection, is introduced, which can be fabricated at low cost by using microwave-assisted batch synthesis techniques.  相似文献   

9.
Dan Luo  Fei Chen  Yu-Qi Feng 《Talanta》2009,77(5):1701-3016
A method was developed for the determination of Δ9-Tetrahydrocannabinol (THC) in saliva by polymer monolith microextraction (PMME) combined with gas chromatography-mass spectrometry. The poly(methacrylic acid-co-ethylene glycol dimethacrylate) (p(MAA-co-EGDMA)) monolithic capillary column was selected as the extraction medium of PMME, which showed high extraction capacity towards THC in saliva. To reach optimum PMME extraction performance, several PMME parameters were investigated, including matrix pH, flow rate for extraction, sampling volume and elution solvent. Under the optimal conditions, good extraction efficiency was obtained with no matrix interference in the process of extraction and the subsequent GC-MS analysis. In the selected-ion monitoring (SIM) mode, the limit of detection (LOD) for THC was 0.68 ng/mL. The linearity range of the method was 3-300 ng/mL. Excellent reproducibility of the method was exhibited by intra- and inter-day precisions, yielding the relative standard deviations (R.S.D.s) less than 12%; recoveries higher than 89%. The proposed method was proved to be rapid, sensitive, and competently applied to the determination of THC in saliva samples.  相似文献   

10.
A qualitative and quantitative analytical method was developed for the simultaneous determination of Δ9‐tetrahydrocannabinol (THC), 11‐hydroxy‐Δ9‐tetrahydrocannabinol (11‐OH‐THC) and l1‐nor‐9‐carboxy‐Δ9‐tetrahydrocannabinol (THC‐COOH) in whole blood. The samples were prepared by solid‐phase extraction followed by ultra‐performance liquid chromatography/tandem mass spectrometry (UPLC/MS/MS) analysis using positive ion electrospray ionization and multiple reaction monitoring. The chromatographic separation was performed with an Acquity UPLC® HSS T3 (50 × 2.1 mm i.d., 1.8 µm) reversed‐phase column using a methanol/2 mM ammonium formate (formic acid 0.1%) gradient in a total run time of 9.5 min. MS/MS detection was achieved with two precursor‐product ion transitions per substance. The method was fully validated, including selectivity and capacity of identification, according to the identification criteria (two transitions per substance, signal‐to‐noise ratio, relative retention time and ion ratio) without the presence of interferences, limit of detection (0.2 µg/L for THC and 0.5 µg/L for 11‐OH‐THC and THC‐COOH), limit of quantitation (0.5 µg/L for all cannabinoids), recovery (53–115%), carryover, matrix effect (34‐43%), linearity (0.5‐100 µg/L), intra‐assay precision (CV < 10% for the relative peak area ratios and <0.1% for the relative retention time), inter‐assay accuracy (mean relative error <10%) and precision (CV <11%). The method has already been successfully used in proficiency tests and subsequently applied to authentic samples in routine forensic analysis. Copyright © 2011 John Wiley & Sons, Ltd.  相似文献   

11.
We have applied sweeping micellar electrokinetic chromatography (sweeping-MEKC) to the simultaneous determination of Delta(9)-tetrahydrocannabinol (THC) and its major metabolites, 11-hydroxy-Delta(9)-tetrahydrocannabinol (THC-OH) and 11-nor-9-carboxy-Delta(9)-tetrahydrocannabinol (THC-COOH). We monitored the effects of several of the sweeping-MEKC parameters, including the proportion of organic modifier, the concentration of sodium dodecyl sulfate (SDS), the pH, and the sample injection volume, to optimize the separation process. The optimal buffer for the analysis of the three analytes was 25 mM citric acid/disodium hydrogenphosphate (pH 2.6) containing 40% methanol and 75 mM SDS. Under the optimized separation parameters, the enrichment factors for THC, THC-COOH, and THC-OH when using sweeping-MEKC (relative to MEKC) were 77, 139, and 200, respectively. The limits of detection (LODs) for the three compounds in standard solutions ranged from 3.87 to 15.2 ng/mL. We combined the sweeping-MEKC method with solid-phase extraction to successfully detect THC, THC-COOH, and THC-OH in human urine with acceptable repeatability. The LODs of these analytes in urine samples ranged from 17.2 to 23.3 ng/mL. Therefore, this sweeping-MEKC method is useful for determining, with high sensitivity, the amounts of THC and its metabolites in the urine of suspected THC users.  相似文献   

12.
Curcumin (CUR) is the major active component of turmeric and plays an important role in the prevention and treatment of many chronic diseases such as respiratory and neurodegenerative disease. In the present work, a rapid and simple LC–MS/MS method was developed to investigate the pharmacokinetics and tissue distribution of CUR and its metabolites in mice after intravenous administration of CUR (20 mg/kg). The results showed that the values of AUC0–∞ were 107.0 ± 18.3, 6.0 ± 1.2 and 12.0 ± 4.0 (mg/L) min, and those for t1/2z were 32.4 ± 10.8, 6.4 ± 2.4 and 5.6 ± 1.8 min for CUR, dihydrocurcumin (DHC) and tetrahydrocurcumin (THC) in plasma, respectively. CUR and THC could be detected in liver while CUR and DHC were detected in kidney. Only CUR was detected in brain. These findings indicated that THC was the main metabolite of CUR in plasma. The exposure of CUR in plasma was 6‐fold greater than that in liver, kidney and brain.  相似文献   

13.
In order to detect hashish intake, urine, blood and serum were analysed for the main components of hashish, i.e., tetrahydrocannabinol (THC), cannabidiol, cannabinol and the decomposition product of THC, THC-carboxylic acid. After extraction and silylation, the samples were analysed by gas chromatography-mass spectrometry with multiple ion detection. The Emit-st-system is used as a pretest for urine.  相似文献   

14.
A simple, isocratic high performance liquid chromatography system (HPLC) with electrochemical detection (EC) was used to study Cannabis constituents. Several Cannabis extracts and reference standards were examined. A total of eleven constituents were separated, and three major cannabinoids; Δ8, Δ9 tetrahydrocannabinol (THC) and cannabidiol (CBD) were identified. A linear relationship was established for the quantitation of the halucinogenic constituent Δ9 THC. Minor contaminants in Δ9 THC reference standard, which were not detected by gas chromatography (GC) were detected for the first time. The detection limits of Δ9 THC and related cannabinoids were in the low nanogram range (2–20 ng).  相似文献   

15.
A simple, specific, and precise high-performance liquid chromatographic method has been developed for the simultaneous determination of ofloxacin (OFX), tetrahydrozoline hydrochloride (THC), and prednisolone acetate (PAC) in ophthalmic suspension using propylparaben (POP) as the internal standard. The mobile phase consists of 0.05 M phosphate buffer-acetonitrile (65:35, v/v), and the pH is adjusted to 2.7 with orthophosphoric acid. A column containing octadecyl silane chemically bonded to porous silica particles (Waters Spherisorb, 5 microm ODS 1, 4.6 x 150 mm) is used as the stationary phase. The detection is carried out using a variable wavelength UV-vis detector set at 210 nm for OFX and THC and 254 nm for POP (internal standard) and PAC. The solutions are chromatographed at a constant flow rate of 1.2 mL/min. Retention times for OFX, THC, POP, and PAC are approximately 2.5, 4.5, 7.8, and 9.5 min, respectively. The relative retention times are approximately 0.14 min for OFX, 0.35 min for THC, 1.00 min for POP, and 1.22 min for PAC. The linearity range and percent recoveries for OFX, THC, and PAC are 24-120, 4-16, and 16-80 microg/mL and 100.48%, 100.34%, and 100.21%, respectively.  相似文献   

16.
Cannabis is not only a widely used illicit drug but also a substance which can be used in pharmacological therapy because of its analgesic, antiemetic, and antispasmodic properties. A very rapid and sensitive method for determination of ?9-tetrahydrocannabinol (THC), the principal active component of cannabis, and two of its phase I metabolites in plasma has been developed and validated. After solid-phase extraction of plasma (0.2 mL), the clean extracts were analyzed by tandem mass spectrometry after a 5-min liquid chromatographic separation. The linear calibration ranges were from 0.05 to 30 ng?mL?1 for THC and 11-nor-?9-carboxy-tetrahydrocannabinol (THC-COOH) and from 0.2 to 30 ng?mL?1 for ?9-(11-OH)-tetrahydrocannabinol (11-OH-THC). Imprecision and inaccuracy were always below 7 and 12 % (expressed as relative standard deviation and relative error), respectively. The method has been successfully applied to determination of the three analytes in plasma obtained from healthy volunteers after oral administration of 20 mg dronabinol.  相似文献   

17.
张爱芝  王全林  莫世杰# 《色谱》2010,28(11):1015-1019
建立了超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定食用油中δ-9-四氢大麻酚(THC)、大麻酚(CBN)和大麻二酚(CBD)的方法。目标分析物经甲醇提取、中性氧化铝固相萃取柱净化后,采用UPLC-MS/MS分离和检测。实验以氘代四氢大麻酚(THC-D3)为内标物,采用同位素内标法定量。在3个添加水平下,目标物的平均回收率为68.0%~101.6%,相对标准偏差为7.0%~20.1%。方法检出限为0.06~0.17 μg/kg,定量限为0.20~0.52 μg/kg。该方法能够满足食用油中痕量四氢大麻酚、大麻酚和大麻二酚检测的需要。  相似文献   

18.
Oral fluid (OF) is an alternative biological matrix for monitoring cannabis intake in drug testing, and drugged driving (DUID) programs, but OF cannabinoid test interpretation is challenging. Controlled cannabinoid administration studies provide a scientific database for interpreting cannabinoid OF tests. We compared differences in OF cannabinoid concentrations from 19 h before to 30 h after smoking a 6.8 % THC cigarette in chronic frequent and occasional cannabis smokers. OF was collected with the Statsure Saliva Sampler? OF device. 2D-GC-MS was used to quantify cannabinoids in 357 OF specimens; 65 had inadequate OF volume within 3 h after smoking. All OF specimens were THC-positive for up to 13.5 h after smoking, without significant differences between frequent and occasional smokers over 30 h. Cannabidiol (CBD) and cannabinol (CBN) had short median last detection times (2.5–4 h for CBD and 6–8 h for CBN) in both groups. THCCOOH was detected in 25 and 212 occasional and frequent smokers’ OF samples, respectively. THCCOOH provided longer detection windows than THC in all frequent smokers. As THCCOOH is not present in cannabis smoke, its presence in OF minimizes the potential for false positive results from passive environmental smoke exposure, and can identify oral THC ingestion, while OF THC cannot. THC?≥?1 μg/L, in addition to CBD?≥?1 μg/L or CBN?≥?1 μg/L suggested recent cannabis intake (≤13.5 h), important for DUID cases, whereas THC?≥?1 μg/L or THC?≥?2 μg/L cutoffs had longer detection windows (≥30 h), important for workplace testing. THCCOOH windows of detection for chronic, frequent cannabis smokers extended beyond 30 h, while they were shorter (0–24 h) for occasional cannabis smokers.  相似文献   

19.
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  
彭兴盛 《色谱》1998,16(2):170-172
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   

20.
Non-aqueous capillary electrophoresis with electrochemical detection (NACE-ED) was applied to the determination of cannabinoids in hair. The effect of different electrolyte compositions on the selectivity of the separation of tetrahydrocannabinol (THC), cannabinol (CBN), cannabidiol (CBD) and tetrahydrocannabinol carboxylic acid (THCA) was studied. Complete electrophoretic resolution was obtained using a strongly basic background electrolyte consisting of 5 mM sodium hydroxide dissolved in acetonitrile-methanol (1:1). Electrochemical detection yielded well defined signals in the oxidation mode. In order to obtain low limits of detection experimental parameters, which determine the sensitivity and the noise level, were optimized. A crucial parameter for sensitive measurements using a wall-tube flow cell as end-column detector is the distance between the capillary outlet and the working electrode. The highest signal-to-noise ratio using a 50 microm I.D. capillary was obtained at a distance of 25 microm. When the capillary outlet was moved away from the working electrode, thus reducing the strength of the separation field present at the working electrode, a large low frequency noise developed. This rise was attributed to disturbances of the hydrodynamic pattern in the flow cell. Analytical aspects such as sensitivity, reproducibility and selectivity were addressed in this work. The precision of NACE-ED regarding migration time and peak height for a sample containing 1 microg/ml THC was 0.4% and 1.1% (RSD), respectively (n=5). The calibration curve was linear for concentrations ranging between 0.1 and 10 microg/ml (r=0.998). The limit of detection for THC was 37 ng/ml, which is almost two orders of magnitude lower when compared with on-column UV detection. The method was evaluated using hair samples containing cannabinoids as sample material.  相似文献   

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