Fully Automated Determination of Cannabinoids in Hair Samples using Headspace Solid-Phase Microextraction and Gas Chromatography–Mass Spectrometry (original) (raw)
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Analytica Chimica Acta, 2010
The development of an analytical method for the determination of 9 -tetrahydrocannabinol (THC), cannabidiol (CBD) and cannabinol (CBN) in samples of human hair is described. Samples were subjected to a procedure based on the combination of headspace solid-phase microextraction (HS-SPME) with gas chromatography linked with mass spectrometry operating in tandem mode (GC-MS/MS). A 10 mg aliquot of sample was firstly decontaminated using petroleum ether, deionized water and dichloromethane (2 mL of each solvent), for 10 min under sonication, and then digested in alkaline solution (1 mol L −1 NaOH). The method variables evaluated were pH, mass of hair, fiber type, extraction temperature, desorption time, ionic strength, pre-equilibrium time and extraction time. Parameters concerning operation of the tandem mode MS/MS were also assessed and optimized. Validation of the method demonstrated excellent linearity in the range 0.1-8.0 ng mg −1 , with regression coefficients better than 0.994. Precision was determined using two different concentrations (upper and lower limits of the linear range), and RSD values were between 6.6 and 16.4%. Absolute recoveries (measured in triplicate) were in the range 1.1-8.7%, and limits of detection and quantification were 0.007-0.031 ng mg −1 and 0.012-0.062 ng mg −1 , respectively. The LOQ for THC (0.062 ng mg −1 ) was below the cut-off value (LOQ ≤ 0.1 ng mg −1 ) established by the Society of Hair Testing (SOHT), the Society of Toxicological and Forensic Chemistry (STFCh) and the Société Franç aise de Toxicologie Analytique (SFTA). The optimized SPME method was applied in analysis of hair samples from Cannabis drug users, showing that CBN and CBD were present in all samples analyzed.
Arch Pharm Research, 2005
An analytical method was developed for evaluating the cannabidiol (CBD), cannabinol (CBN), and ALtetrahydrocannabinol (A9-THC) level in human hair using gas chromatography-mass spectrometry (GC-MS). Hair samples (50 mg) were washed with isopropyl alcohol and cut into small fragments (< 1 mm). After adding a deuterated internal standard, the hair samples were incubated in 1.0 M NaOH for 10 min at 95~ The analytes from the resulting hydrolyzed samples were extracted using a mixture of n-hexane-ethyl acetate (75:25, v/v). The extracts were then evaporated, derivatized, and injected into the GC-MS. The recovery ranges of CBD, CBN, and ~?-THC at three concentration levels were 37.9-94.5% with good correlation coefficients (r 2 >0.9989). The intra-day precision and accuracy ranged from-9.4% to 17.7%, and the inter-day precision and accuracy ranged from-15.5% to 14.5%, respectively. The limits of detection (LOD) for CBD, CBN, and A9-THC were 0.005, 0.002, and 0.006 ng/mg, respectively. The applicability of this method of analyzing the hair samples from cannabis abusers was demonstrated.
Detection of Δ9-tetrahydrocannabinol (THC) in hair using GC–MS
Egyptian Journal of Forensic Sciences, 2014
Detection of drugs from hair samples has become an imperative technique in forensic toxicological analysis. In this study, hair samples were collected from 20 cannabis users undergoing treatment at a rehabilitation center at different time intervals. Hair samples were cleaned and digested, followed by extraction and quantification of THC by GC-MS. At LOD of 0.1 ng/mg of THC, the concentration ranged from 0.16 to 2.3 ng/mg (mean, 0.95 ng/mg). Results indicate that THC is detectable after 3 months of last drug intake.
Forensic Toxicology, 2014
When narcotics police officers or other persons handling drug materials at work are suspected of consuming drugs, hair analysis may be useful to prove or refute such suspicion. However, it is known for many drugs that differentiation between actual drug use and external contamination can be challenging or sometimes impossible. This study evaluated the extent of external contamination caused by handling of synthetic cannabinoidcontaining materials under realistic conditions in a forensic laboratory. Hair samples of laboratory staff were systematically analyzed for synthetic cannabinoids with a validated liquid chromatography-tandem mass spectrometry method after a large quantity of seized ''legal high'' products was analyzed in our laboratory. Furthermore, hair samples of laboratory staff not directly in contact with the drug materials and close relatives of exposed subjects were analyzed to check for cross contamination. All samples of persons who were in direct contact with drug materials tested positive for at least one synthetic cannabinoid. Concentrations ranged from trace amounts up to a maximum of 170 pg/mg (JWH-210), and roughly reflected the duration and intensity of exposure. Unexpectedly, subjects without direct contact with drug material also showed measurable concentrations of synthetic cannabinoids in hair. Concentrations caused by contamination were within the typical range found in known users of these drugs and could lead to false positive results and incorrect conclusions. Therefore, we recommend that body fluids should be simultaneously analyzed to unambiguously prove use of these drugs.
Drug Testing and Analysis, 2009
A quantitative analytical procedure for the determination of 9 -tetrahydrocannabinol (THC) in hair has been developed and validated using liquid chromatography with tandem mass spectral detection (LC-MS/MS). Specimens that were determined as containing cannabinoids following immunoassay testing were quantified using solid-phase extraction followed by liquid chromatographic separation and tandem mass spectral detection in positive electrospray ionization mode. For confirmation, two transitions were monitored and one ratio determined. Samples being reported as positive were required to have both transitions present, the ratio of quantifying transition to qualifying transition being within 20% of that determined from known calibration standards. The limit of quantitation and the limit of detection was 10 pg/mg. The percentage recovery of the THC from hair at 20 pg/mg was 56% and a matrix effect of the hair showed an ion suppression percentage of −51%. The immunochemical screening method was performed following a rapid aqueous extraction, requiring only 10 mg of hair; the confirmatory procedure required 20 mg of hair. The methods were applied to proficiency specimens from the Society of Hair Testing, which had been
Hair analysis for Δ9-THC, Δ9-THC-COOH, CBN and CBD, by GC/MS-EI
Forensic Science International, 2002
A sensitive analytical method was developed for quantitative analysis of D 9 -tetrahydrocannabinol (D 9 -THC), 11-nor-D 9tetrahydrocannabinol-carboxylic acid (D 9 -THC-COOH), cannabinol (CBN) and cannabidiol (CBD) in human hair. The identification of D 9 -THC-COOH in hair would document Cannabis use more effectively than the detection of parent drug (D 9 -THC) which might have come from environmental exposure.
Journal of Chromatography B, 2012
Herbal mixtures of the "Spice"-type contain a variety of synthetic cannabinoids. To prove the contact of a person with synthetic cannabinoids in a previous period of up to several months, hair testing is ideally suited. A rapid, simple and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) assay was developed to determine 22 synthetic cannabinoids in human hair. The synthetic cannabinoids JWH-007, JWH-015, JWH-018, JWH-019, JWH-020, JWH-073, JWH-081, JWH-122, JWH-200, JWH-203, JWH-210, JWH-250, JWH-251, JWH-398, AM-694, AM-2201, methanandamide, RCS-4, RCS-4 ortho isomer, RCS-8, WIN 48,098 and WIN 55,212-2 were extracted from 50 mg hair by 3-h ultrasonification in ethanol. The extracts were analysed on a triple-quadrupole linear ion trap mass-spectrometer in scheduled multiple reaction monitoring mode (sMRM). The method was fully validated and proved to be accurate, precise, selective and specific with satisfactory linearity within the calibrated range and a lower limit of quantification of 0.5 pg/mg for 20 compounds. Authentic hair samples from chronic consumers showed the presence of two to six synthetic cannabinoids in the same segment. In the first segment, concentrations of up to 78 pg/mg JWH-081 were present. In segmented hair, the concentrations of most substances increased from the first (proximal) to the third segment. The highest concentration was ca. 1100 pg/mg JWH-081. The results of segmental hair analysis in chronic users suggest incorporation of the drugs in head hair via side-stream smoke condensation as a major route. In summary, the method can be used to prove the contact with herbal mixtures containing synthetic cannabinoids and thus contributes to an efficient abstinence control.
BMC Chemistry
Cannabis products (marijuana, weed, hashish) are among the most widely abused psychoactive drugs in the world, due to their euphorigenic and anxiolytic properties. Recently, hair analysis is of great interest in analytical, clinical, and forensic sciences due to its non-invasiveness, negligible risk of infection and tampering, facile storage, and a wider window of detection. Hair analysis is now widely accepted as evidence in courts around the world. Hair analysis is very feasible to complement saliva, blood tests, and urinalysis. In this review, we have focused on state of the art in hair analysis of cannabis with particular attention to hair sample preparation for cannabis analysis involving pulverization, extraction and screening techniques followed by confirmatory tests (e.g., GC-MS and LC-MS/MS). We have reviewed the literature for the past 10 years' period with special emphasis on cannabis quantification using mass spectrometry. The pros and cons of all the published methods have also been discussed along with the prospective future of cannabis analysis.
This paper describes the analysis of cannabinoids in the hair of the user of the narcotic type of marijuana (Cannabis sativa L), using the technique Gas Chromatography Mass Spectroscopy (GCMS) and the validation of the method used. This research was conducted through experiments. Samples were taken from users of narcotic type of marijuana, found in Al-Kamal Sibolangit Rehabilitation Centre, North Sumatra, Indonesia. Marijuana plants were taken from the evidence in Forensic Laboratory of Medan Branch Police. Extraction is done through maceration by sonication at 42 KHz and using methanol – 2 propanol (1:1), kloroform, and petroleum benzene each of 2 ml for 5 minutes. Testing is done with fast blue salt B test and show there is a precipitate Violet. Optimal results obtained at a temperature of 50°C extraction. Identification is done with Thin Layer Chromatography (TLC) in the mobile phase of toluene and n-hexane (1:1) under alkaline conditions of pH 9,5, followed by GC MS techniques for sixteen (16) minutes. The results are contained compounds of cannabidiol, cannabinol, and ∆ 9 THC (Tetrahydrocannabinoid) with concentrations ranging from 0.25 up to 2.82 ng/mg in the hair of the user. Validation of GC MS method for the compounds of cannabidiol, cannabinol, and ∆ 9 THC produces an accuracy value with %recovery is 103,83, 102,67, and 101,17 respectively. Precision test produces a value of Relatif Standard Deviation (RSD) = 1,3058%, 0,8997%, dan 0,8997% respectively. Linearity test generate r value each of the regression is 0,922, 0,955, and 0,921. Limits of Detection (LOD) is obtained 0,000168 ng/mg, 0,000117 ng/mg, and 0,000164 respectively. Limits of Quantification (LOQ) is 0,00056 ng/mg, 0,00039 ng/mg, and 0,00054 ng/mg respectively. This indicates that the modification process of extraction and GC MS techniques used could produce cannabinoid compounds (cannabidiol, cannabinol, and ∆ 9 THC) in hair samples quickly and accurately.