Determination of Selected Opiates in Hair Samples Using Microextraction by Packed Sorbent: A New Approach for Sample Clean-up

Abstract

Abstract In this article the development and validation of an analytical method using microextraction by packed sorbent (MEPS) to determine tramadol (TRM), codeine (COD), morphine (MOR), 6-acetylcodeine (6-AC), 6-monoacetylmorphine (6-MAM) and fentanyl (FNT) in hair samples by gas chromatography coupled to tandem mass spectrometry (GC–MS-MS) is presented. The MEPS used a mixed mode sorbent, and the steps for sample cleanup were conditioning (three cycles of 250 μL of methanol and three cycles of 250 μL formic acid 2%); sample load (15 cycles of 150 μL); wash (150 μL of 3.36% formic acid); and elution (eight cycles of 100 μL of ammonium hydroxide 2.36% (in methanol)). Linearity was obtained from the lower limit of quantitation (LLOQ) up to 5 ng/mg, with all target compounds revealing determination coefficients >0.99. The LLOQs achieved were 0.01 ng/mg for TRM, COD and 6-AC, and 0.025 ng/mg for MOR, 6-MAM and FNT. The recoveries ranged from 74 to 90% (TRM), 51 to 59% (COD), 22 to 36% (MOR), 69 to 99% (6-AC), 53 to 61% (6-MAM) and 75 to 86% (FNT). Precision and accuracy revealed coefficients of variation typically below 15% and relative errors within a ±15% interval, respectively. This new approach has proven to be an excellent alternative to classic procedures, reducing the volumes of organic solvents required.