A high-throughput method based on microwave-assisted extraction and liquid chromatography–tandem mass spectrometry for simultaneous analysis of amphetamines, ketamine, opiates, and their metabolites in hair

Abstract

A total sample-preparation and analysis time of 50 min is required for the high-throughput method of hair analysis proposed in this paper. The method is applicable to analysis of drugs commonly used in Asia, and their metabolites--methamphetamine (MA), amphetamine (AMP), methylenedioxymethamphetamine (MDMA), methylenedioxyamphetamine (MDA), ketamine (K), norketamine (NK), dehydronorketamine (DHNK), 6-acetylmorphine (6-AM), morphine (MOR), and codeine (COD). Cut and weighed hair (10 mg) was incubated for 3 min with methanol-trifluoroacetic acid (TFA) during microwave-assisted extraction (MAE) at 700 W. The incubation solution was evaporated, the residue was reconstituted in deionized water-methanol, 99:1 (v/v), and 20 μL was injected on to a core-shell column (50 × 4.6 mm, 2.6 μm particle size) for liquid chromatographic-tandem mass spectrometric (LC-MS-MS) analysis. Gradient elution separation was performed in 8 min at a flow rate of 1 mL min(-1). No signal interfering with any of the analytes was found in fourteen blank hair samples from different sources. The limits of detection and quantification were 0.5 pg mg(-1) and 2.0 pg mg(-1), respectively, for MA, AMP, MDMA, MDA, K, NK, and DHNK, and 2.0 pg mg(-1) and 5.0 pg mg(-1), respectively, for 6-AM, MOR and COD. The linear range was between the LOQ and 1000 pg mg(-1), and the correlation coefficients were all greater than 0.999. Investigation of matrix effects revealed that all the analytes were suppressed by less than 20% and the standard deviation (SD) was always less than 7%. Recovery was always greater than 90% and the SD for each compound was less than 6%. Precision and accuracy for each analyte were within 15%. Eight authentic hair specimens from known drug abusers were successfully analyzed. Compared with traditional overnight incubation methods, the rapid 3-min extraction time achieved similar or greater extraction yields. Sample preparation by MAE was a reliable procedure for extraction of the analytes from hair but substantially simpler and faster than other methods.

Maternal and Neonatal Hair and Breast Milk in The Assessment of Perinatal Exposure to Drugs of Abuse

“…To test for the high number of drugs and metabolites in hair samples, pharmacotoxicology laboratories are required to update analytical procedures, in order to achieve rapid, simple and sensitive analyses with reduced sample preparation and instrumental processing, to finally increase overall sample-throughput. Different methods have been proposed for testing class-specific groups of compounds [66,69,[72][73][74][77][78][79], but only a few articles describe extensive analysis of multiclass drugs [60,61,[63][64][65]67,68,75,76,80] with some including also methods for THC quantification [62,70,71].…”

“…Currently, triple quadrupole type mass spectrometers are the most widely used for LC-MS testing and have become the preferred analytical instruments for drugs of abuse detection [65,[69][70][71][73][74][75][76][77][78]. Triple quadrupoles can perform single quadrupole experiments such as full scan and selected ion monitoring (SIM) experiments and have the capability of specialized tandem (MS/MS) scan modes such as product ion scanning, precursor ion scanning, constant neutral loss and multiple reaction monitoring.…”

“…Due to the small amount of hair specimen usually available for analysis, multianalyte methods are recommended, saving time, costs and amount of specimen required. To date, several analytical procedures for testing of drugs in hair have been reported, with most of them, focused on the validation of methods for the detection of drugs of abuse usually found in hair [60][61][62][63][64][65][66][67][68][69][70][71][72][73][74][75][76][77][78][79]. The most important validation parameters (recovery, intra-assay and interassay precision and accuracy and limit of detection and quantification) as a function of analytical method and matrix extraction for different drugs of abuse determined in hair are summarized in Table 1.…”

Detection of New Psychoactive Substances

“…Its abuse was recognized in the United States since the beginning of the 1980s and started to be noticed in Europe in the 1990s [4]. The analytical techniques most frequently used to detect ketamine and norketamine in hair were GC-MS [15,16,18,27,34,35] and LC-MS/MS (or LC-HRMS) [17,20,32]. In this form, it can be administered orally, inhaled, snorted, or smoked.…”

Determination of amphetamines in biological samples using electro enhanced solid-phase microextraction-gas chromatography

“…Prior to chromatographic analysis, a sample preparation step is required to enrich and separate the amphetamines from biological fluids.. For this purpose, solid-phase extraction [5][6][7][8] and liquid-liquid extraction [9][10][11] are often used. .…”