Development and Application of Stir Bar Sorptive Extraction with Polyurethane Foams for the Determination of Testosterone and Methenolone in Urine Matrices

Abstract

This work describes the development, validation, and application of a novel methodology for the determination of testosterone and methenolone in urine matrices by stir bar sorptive extraction using polyurethane foams [SBSE(PU)] followed by liquid desorption and high-performance liquid chromatography with diode array detection. The methodology was optimized in terms of extraction time, agitation speed, pH, ionic strength and organic modifier, as well as back-extraction solvent and desorption time. Under optimized experimental conditions, convenient accuracy were achieved with average recoveries of 49.7 8.6% for testosterone and 54.2 ± 4.7% for methenolone. Additionally, the methodology showed good precision (<9%), excellent linear dynamic ranges (>0.9963) and convenient detection limits (0.2-0.3 μg/L). When comparing the efficiency obtained by SBSE(PU) and with the conventional polydimethylsiloxane phase [SBSE(PDMS)], yields up to four-fold higher are attained for the former, under the same experimental conditions. The application of the proposed methodology for the analysis of testosterone and methenolone in urine matrices showed negligible matrix effects and good analytical performance.

Stir-bar sorptive extraction: 15 years making sample preparation more environment-friendly

“…The PU foams proposed were shown to be a promising, advantageous polymeric phase, when compared with SBSE(PDMS), using both sampling modes (HS and immersion) to monitor priority targets having a wide range of polarity (e.g., triazinic herbicides and metabolites in water, roasted coffee volatiles, acidic pharmaceuticals and hormones in biological fluids) [65][66][67].…”

Automated and sensitive determination of four anabolic androgenic steroids in urine by online turbulent flow solid-phase extraction coupled with liquid chromatography–tandem mass spectrometry: A novel approach for clinical monitoring and doping control

“…Meanwhile, the operative error is hard to be avoided. In order to simplify the pretreatment procedure and improve the method sensitivity, some new techniques such as molecular imprinted polymer solid phase extraction (SPE) [25,26], solid phase microextraction (SPME) [27], stir bar microextraction (SBME) [28] and online SPE [29,30], have also been applied to determine AAS in diverse biological samples.…”

Quantitative analysis of total methenolone in animal source food by liquid chromatography‐tandem mass spectrometry

“…All samples were extracted, purified and analyzed as before. It was indicated that the recovery of all meat or egg/milk samples was above 90% (Table 4), higher than that in previous study 14 . The high recovery of methenolone may be attributed to the optimized sample preparation and HPLC‐MS/MS determination process.…”

“…In another study, LC‐MS/MS was used to directly detect the glucuronide‐conjugated metabolite of methenolone in human urine with a LOD at 1.0 ng/ml and a high recovery rate of 95% 13 . Sequeiros et al 14 developed an HPLC method by stir bar sorptive extraction using polyurethane foams with a lower LOD (0.2 ng/ml) but a less recovery (54.2%). Further, Guo et al 8 improved the LC‐MS/MS method by using Turboflow C18‐P SPE for purification, and better sensitivity (LOD, 0.01 ng/ml; low limit of quantification [LOQ], 0.1 ng/ml) was obtained for the online testing of human urine samples.…”