Fabric-Phase Sorptive Membrane Array As a Noninvasive In Vivo Sampling Device For Human Exposure To Different Compounds.

This study introduces an innovative device for the noninvasive sampling and chromatographic analysis of different compounds present in exhaled breath aerosol (EBA). The new sampling device, especially in light of the recent COVID-19 pandemic that forced many countries to impose mandatory facemasks, allows an easy monitoring of the subject's exposure to different compounds they may come in contact with, actively or passively. The project combines the advantages of a fabric-phase sorptive membrane (FPSM) as an in vivo sampling device with a validated LC-MS/MS screening procedure able to monitor more than 739 chemicals with an overall analysis time of 18 min. The project involves the noninvasive in vivo sampling of the EBA using an FPSM array inserted inside an FFP2 mask. The study involved 15 healthy volunteers, and no restrictions were imposed during or prior to the sampling process regarding the consumption of drinks, food, or drugs. The FPSM array-LC-MS/MS approach allowed us to effectively exploit the advantages of the two complementary procedures (the convenient sampling by an FPSM array and the rapid analysis by LC-MS/MS), obtaining a powerful and green tool to carry out rapid screening analyses for human exposure to different compounds. The flexible fabric substrate, the sponge-like porous architecture of the high-efficiency sol-gel sorbent coating, the availability of a large cache of sorbent coatings, including polar, nonpolar, mixed mode, and zwitterionic phases, the easy installation into the facemask, and the possibility of sampling without interrupting regular activities provide FPSMs unparalleled advantages over other sampling techniques, and their applications are expected to expand to many other clinical or toxicological studies.

An FPSE-HPLC-PDA method for rapid determination of solar UV filters in human whole blood, plasma and urine.

This paper reports a novel fabric phase sorptive extraction-high performance liquid chromatography-photodiode array detection (FPSE-HPLC-PDA) method for the simultaneous extraction and analysis of six benzophenone derivative UV filters including benzophenone (BZ); 5-benzoyl-4-hydroxy-methoxybenzenesulfonic acid (BP-4); bis(4-hydroxyphenyl)methanone (4-DHB); bis(2,4-dihydroxyphenyl)methanone (BP-2); (2,4-dihydroxybenzophenone) (BP-1) and 2,2'-dihydroxy-4-methoxybenzophenone (DHMB) in human whole blood, plasma and urine samples. Chromatographic separation method was conducted using a Spherisorb ODS 1 (C18) column in isocratic elution mode with a run time <25 min. The FPSE-HPLC-PDA method was validated in the range from 0.1 to 10 µg/mL for all the UV filter compounds. Propyl 4-hydroxybenzoate (also known as propyl paraben) was used as the internal standard (IS). The limit of quantification was found to be 0.1 µg/mL and the weighted-matrix matched standard calibration curves of six UV filters showed a good linearity up to a concentration of 10 µg/mL. This new approach exhibits high potential for direct adaptation as a rapid, robust and green analytical tool for several applications, e.g. in the current sample preparation practices used in many bioanalytical fields including pharmacokinetics (PK), pharmacodynamics (PD), therapeutic drug monitoring (TDM), clinical and forensic toxicology, disease diagnosis and drug discovery. Additionally, in the present work was highlighted that applying innovative extraction and clean up procedures before instrumental analysis by means of a well-known, rugged, cheap, and diffused configurations (e.g. HPLC-PDA), could be possible to validate methods that shows analytical performances comparable to more expensive and complex instrumentations (e.g. LC-MS/MS) that require trained personnel, high maintenance costs and a deep knowledge of analytical problems that could be encountered.

Comparison between Exhaustive and Equilibrium Extraction Using Different SPE Sorbents and Sol-Gel Carbowax 20M Coated FPSE Media.

This paper reports the performance comparison between the exhaustive and equilibrium extraction using classical Avantor C18 solid phase extraction (SPE) sorbent, hydrophilic-lipophilic balance (HLB) SPE sorbent, Sep-Pak C18 SPE sorbent, novel sol-gel Carbowax 20M (sol-gel CW 20M) SPE sorbent, and sol-gel CW 20M coated fabric phase sorptive extraction (FPSE) media for the simultaneous extraction and analysis of three inflammatory bowel disease (IBD) drugs that possess logP values (polarity) ranging from 1.66 for cortisone, 2.30 for ciprofloxacin, and 2.92 for sulfasalazine. Both the commercial SPE phases and in-house synthesized sol-gel CW 20M SPE phases were loaded in SPE cartridges and the extractions were carried out under an exhaustive extraction mode. FPSE was carried out under an equilibrium extraction mode. The drug compounds were resolved using a Luna C18 column (250 mm × 4.6 mm; 5 m particle size) in gradient elution mode within 20 min and the method was validated in compliance with international guidelines for the bioanalytical method validation. Novel in-house synthesized and loaded sol-gel CW 20M SPE sorbent cartridges were characterized in terms of their extraction capability, breakthrough volume, retention volume, hold-up volume, number of the theoretical plate, and the retention factor.