TY - JOUR T1 - Lab-in-syringe automated protein precipitation and salting-out homogenous liquid-liquid extraction coupled online to UHPLC-MS/MS for the determination of beta-blockers in serum. AU - Yıldırım,Sercan, AU - Fikarová,Kateřina, AU - Pilařová,Veronika, AU - Nováková,Lucie, AU - Solich,Petr, AU - Horstkotte,Burkhard, Y1 - 2023/02/17/ PY - 2022/12/02/received PY - 2023/02/09/revised PY - 2023/02/09/accepted PY - 2023/3/16/entrez PY - 2023/3/17/pubmed PY - 2023/3/17/medline KW - Beta-blockers KW - Centrifugation-less protein precipitation KW - Lab-in-syringe automation KW - Salting-out homogenous liquid-liquid extraction KW - Serum SP - 340966 EP - 340966 JF - Analytica chimica acta JO - Anal Chim Acta VL - 1251 N2 - A sample preparation method involving tandem implementation of protein precipitation and salting-out homogenous liquid-liquid extraction was developed for the determination of beta-blockers in serum. The entire procedure was automated using a computer-controlled syringe pump following the Lab-In-Syringe approach. It is based on the denaturation of serum proteins with acetonitrile followed by salt-induced phase separation upon which the proteins accumulate as a compact layer at the interphase of the solutions. The extract is then separated and diluted in-syringe before being submitted to online coupled UHPLC-MS/MS. A 1 mL glass syringe containing a small stir bar for solution mixing at up to 3000 rpm, was used to deal with sample volumes as small as 100 μL. A sample throughput of 7 h-1 was achieved by performing the chromatographic run and sample preparation procedure in parallel. Linear working ranges were obtained for all analytes between 5 and 100 ng mL-1, with LOD values ranging from 0.4 to 1.5 ng mL-1. Accuracy values in the range of 88.2-106% and high precision of <11% RSD suggest applicability for routine analysis that can be further improved using deuterated standards. SN - 1873-4324 UR - https://www.unboundmedicine.com/medline/citation/36925276/Lab_in_syringe_automated_protein_precipitation_and_salting_out_homogenous_liquid_liquid_extraction_coupled_online_to_UHPLC_MS/MS_for_the_determination_of_beta_blockers_in_serum_ DB - PRIME DP - Unbound Medicine ER -