Electrophoresis. 2022 Apr 16. doi: 10.1002/elps.202100389. Online ahead of print.
Cannabinoids are pharmacologically active compounds present in cannabis plants, which have become important research topics in the modern toxicological and medical research fields. Not only is cannabis the most used drug globally, but also cannabinoids have a growing use to treat a series of diseases. Therefore, new, fast, and efficient analytical methods for analyzing these substances in different matrices are demanded. This study developed a new packed-in-tube solid phase microextraction (IT-SPME) method coupled to LC-MS/MS, for the automated microextraction of 7 cannabinoids from human urine. Packed IT-SPME microcolumns were prepared in (508 μm i.d. x 50 mm) stainless-steel hardware; each one required only 12 mg of sorbent phase. Different sorbents were evaluated; fractional factorial design (24-1 ) and a central composite design were employed for microextraction optimization. Under optimized conditions, the developed method was a fast and straightforward approach. Only 250 μL of urine sample was needed, and no hydrolysis was required. The sample pre-treatment included only dilution and centrifugation steps (8 min), while the complete IT-SPME-LC-MS/MS method took another 12 minutes, with a sample throughput of 3 samples h-1 . The developed method presented adequate precision, accuracy and linearity; R2 values ranged from 0.990 to 0.997, in the range of 10 to 1000 ng mL-1 . The lower limits of quantification (LLOQ) varied from 10 to 25 ng mL-1 . Finally, the method was successfully applied to analyze 20 actual urine samples and the IT-SPME microcolumn was re-used over 150 times. This article is protected by copyright. All rights reserved.
Source: ncbi 2