Development of a solid‐phase microextraction LC–MS/MS method for determination of oxidative stress biomarkers in biofluids

Abstract

Recently the connection between oxidative stress and various diseases, including cancer and Alzheimer's, attracts notice as a pathway suitable for diagnostic purposes. 8-Oxo-deoxyguanosine and 8-oxo-deoxyadenosine produced from the interaction of reactive oxygen species with DNA become prominent as biomarkers. Several methods have been developed for their determination in biofluids, including solidphase extraction and enzyme-linked immunosorbent assays. However, still, there is a need for reliable and fast analytical methods. In this context, solid-phase microextraction offers many advantages such as flexibility in geometry and applicable sample volume, as well as high adaptability to high-throughput sampling. In this study, a solid-phase microextraction method was developed for the determination of 8oxo-deoxyguanosine and 8-oxo-deoxyadenosine in biofluids. The extractive phase of solid-phase microextraction consisted of hydrophilic-lipophilic balanced polymeric particles. In order to develop a solid-phase microextraction method suitable for the determination of the analytes in saliva and urine, several parameters, including desorption solvent, desorption time, sample pH, and ionic strength, were scrutinized. Analytical figures of merit indicated that the developed method provides reasonable interday and intraday precisions (<15% in both biofluids) with acceptable accuracy. The method provides a limit of quantification for both biomarkers at 5.0 and 10.0 ng/mL levels in saliva and urine matrices, respectively. K E Y W O R D Sbiofluid analysis, biomarkers, oxidative stress, sample preparation, solid-phase microextraction

Recent applications of microextraction sample preparation techniques in biological samples analysis

“…A 50/30 μm polydimethylsiloxane (PDMS)/divinylbenzene/carboxen fiber was used for the SPME vial headspace (Tummarintra et al, 2020). Kahremanoglu et al (2020) developed an SPME method coupled with LC-MS/MS for analysis of 8-oxo-deoxyguanosine and 8-oxodeoxyadenosine in saliva and urine matrices. The extractive phase of the SPME consisted of hydrophilic-lipophilic balanced polymeric particles.…”

“…The extractive phase of the SPME consisted of hydrophilic-lipophilic balanced polymeric particles. This method provides an LOQ for both biomarkers at 5.0 and 10.0 ng/ml levels in saliva and urine matrices, respectively (Kahremanoglu et al, 2020).…”

A robust ultra‐performance liquid chromatography‐tandem mass spectrometry method for simultaneous determination of 10 components in glutathione cycle

“…Those methods are easy to operate, but with lower separation efficiency and sensitivity, and only focus on a few analytes, such as GSH, and Cys [17][18][19][20][21][22]. In the near decades, several ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) methods were developed to measure the multiple components in GSH cycles and showed higher sensitivity, but with low separation efficiency, isotope internal standards, or incomplete methodological investigations, which limited the promotion and application [23][24][25][26][27][28].…”