Proof-of-concept chemometric approach for environmental forensic sourcing of crude oil samples using SPME-GC-MS.

Environmental exposure to crude oil through seepage and spillage poses risks to the immediate environment and the broader ecosystem as areas along the oil distribution path are affected by the influx of crude petroleum as well as the environmental, economic, and civil unrest that accompanies it. There is a large financial burden associated with the lost resources, including the cost of rehabilitation, and the affected sources of revenue for communities affected by oil spills. As such, it is crucial to determine the responsible parties.

Exploring canine olfactory generalization using odor profile fractions from native crude oils.

Canines are used by both government agencies and industries for their keen olfactory capability as well as selectivity, reliability, versatility, and speed. Within the last decade, canines have been used for the detection of on-shore crude oil. They were previously shown to find these deposits with high accuracy, providing increased confidence with little risk to oil spill response survey teams.

Ionic-liquid/Carbowax 20 M functionalized capsule phase microextraction platform for the extraction of phosphodiesterase-5 inhibitors from human serum and urine prior to their determination by LC-MS.

Capsule phase microextraction (CPME) is an efficient bioanalytical technique that streamlines the sample preparation by integrating the filtration and stirring mechanism directly into the device. A novel composite sorbent designed to be selective towards the target analytes consisting of mixed-mode sorbent chemistry synthesized by sol-gel technology is found promising and superior to the conventional C sorbents. Herein we describe the encapsulation of an ionic liquid (IL)/Carbowax 20M-functionalized sol-gel sorbent (sol-gel IL/Carbowax 20 M) in the lumen of porous polypropylene tubes for the capsule phase microextraction of three phosphodiesterase-5 inhibitors namely avanafil, sildenafil, and tadalafil in human serum and urine samples.

Adapting Fabric Phase Sorptive Extraction as an Innovative Multitool for Sample Transfer and Extraction in Pharmacokinetic Analysis Followed by LC-MS Determination of Levofloxacin in Plasma Samples.

Fabric phase sorptive extraction (FPSE) is a simple microextraction technique that allows analytes to be rescued from matrix components while using a small volume of samples to analyze complex biological systems. This study used FPSE as a microextraction tool and a sample storage and transfer device. Levofloxacin as a model molecule was applied intravenously (IV) to New Zealand male rabbits.

Calibrating canines-a universal detector calibrant for detection dogs.

Since the advent of the Universal Detector Calibrant (UDC) by scientists at Florida International University in 2013, this tool has gone largely unrecognized and under-utilized by canine scent detection practitioners. The UDC is a chemical that enables reliability testing of biological and instrumental detectors. Training a biological detector, such as a scent detection canine, to respond to a safe, non-target, and uncommon compound has significant advantages.

Sol-gel Carbowax 20M-zwitterionic ionic liquid composite sorbent-based capsule phase microextraction device combined with HPLC/post-column derivatization for the determination of lanreotide, a human somatostatin analogue in urine.

In this research, a sol-gel Carbowax 20M-zwitterionic ionic liquid composite sorbent-based capsule phase microextraction (CPME) device was developed in combination with liquid chromatography-post column derivatization for the first ever reported determination of a somatostatin analogue - lanreotide in human urine. The sol-gel Carbowax 20M-zwitterionic ionic liquid composite sorbent was encapsulated in the lumen of a polypropylene capillary tube and characterized by FT-IR spectroscopy and SEM with energy dispersive X-ray spectroscopy (EDS). The main steps of the CPME workflow were optimized to obtain high extraction efficiency for the target analyte.

Selective determination of 2-aminobenzothiazole in environmental water and organic extracts from fish and dust samples.

In the present study, a homemade mixed-mode ion-exchange sorbent based on silica with embedded graphene microparticles is applied for the selective extraction of 2-aminobenzothiazole (NHBT) followed by determination through liquid chromatography coupled to high-resolution mass spectrometry. The sorbent was evaluated for the solid-phase extraction of NHBT from environmental water samples (river, effluent wastewater, and influent wastewater), and NHBT was strongly retained through the selective cation-exchange interactions. Therefore, the inclusion of a clean-up step of 7 mL of methanol provided good selectivity for the extraction of NHBT.

Fabricating a designer capsule phase microextraction platform based on sol-gel Carbowax 20M-zwitterionic ionic liquid composite sorbent for the extraction of lipid-lowering drugs from human urine samples.

A sol-gel Carbowax 20 M/3-[(3-Cholamidopropyl) dimethyl ammonio]-1-propanesulfonate composite sorbent-based capsule phase microextraction device has been fabricated and characterized for the determination of four statins (pravastatin, rosuvastatin, pitavastatin, and atorvastatin) in human urine. The presence of ionizable carboxyl functional groups in statins requires pH adjustment of the sample matrix to ensure that the target molecules are in their protonated form (pH should be 2 units below their pK values) which not only is cumbersome but also risks unintended contamination of the sample. This challenge was addressed by introducing zwitterionic ionic liquid in addition to neutral, polar Carbowax 20 M polymer in the sol-gel-derived composite sorbent.

Dual sorbent coating based magnet-integrated fabric phase sorptive extraction as a front-end to gas chromatography-mass spectrometry for multi-class pesticide determination in water samples.

Magnet-integrated fabric phase sorptive extraction (MI-FPSE) is a sample preparation technique that has proved to be a powerful tool for environmental analysis. The fabrication and application of magnet-integrated dual sorbent-based FPSE membrane prepared by combining two different sol-gel sorbent-coated disks of different polarities together with a magnetic bar inserted between the two membranes to allow the stirring, was examined as novel preparation technique that not required samples pretreatments. The dual sorbent-based sample preparation platforms (made up of poly(tetrahydrofuran) and Carbowax 20M) were used for the extraction of seven classes of pesticides from ambient surface water samples prior to their determination by gas chromatography-mass spectrometry.

Optimization of a Fabric Phase Sorptive Extraction protocol for the isolation of six bisphenols from juice pouches to be analysed by high performance liquid chromatography coupled with diode array detector.

Fabric Phase Sorptive Extraction (FPSE) combined with high pressure liquid chromatography using to diode array detection (HPLC-DAD) was applied for the simultaneous determination of bisphenols (BPA, BPB, BPC, BPE, BPF, BPS) in juice pouches. The FPSE procedure was optimized with regards to the critical parameters that affect the performance of the method including the selection of the FPSE membrane type and size, adsorption time, extraction time, solvent volume desorption, magnetic stirring ratio, and salt addition. The FPSE membrane could be reused up to 14 times.

Multivariate regression modelling for gender prediction using volatile organic compounds from hand odor profiles via HS-SPME-GC-MS.

The efficacy of using human volatile organic compounds (VOCs) as a form of forensic evidence has been well demonstrated with canines for crime scene response, suspect identification, and location checking. Although the use of human scent evidence in the field is well established, the laboratory evaluation of human VOC profiles has been limited. This study used Headspace-Solid Phase Microextraction-Gas Chromatography-Mass Spectrometry (HS-SPME-GC-MS) to analyze human hand odor samples collected from 60 individuals (30 Females and 30 Males).

An integrated automatic lab-in-syringe sol-gel coated foam microextraction platform as a front-end to high performance liquid chromatography for the migration studies of bisphenol A.

The proof-of-concept of an integrated automatic foam microextraction lab-in-syringe (FME-LIS) platform coupled to high performance liquid chromatography is presented. Three different sol-gel coated foams were synthesized, characterized, and conveniently packed inside the glass barrel of the LIS syringe pump, as an alternative approach for sample preparation, preconcentration and separation. The proposed system efficiently combines the inherent benefits of lab-in-syringe technique, the good features of sol-gel sorbents, the versatile nature of foams/sponges, as well as the advantages of automatic systems.

Design and development of second-generation fabric phase sorptive extraction membranes: Proof-of-concept for the extraction of organophosphorus pesticides from apple juice prior to GC-MS analysis.

In this work, different sol-gel sorbent-coated second-generation fabric phase sorptive extraction (FPSE) membranes were synthesized using titania-based sol-gel precursors. The proposed membranes were tested for their efficiency to extract eleven selected organophosphorus pesticides (OPPs) from apple juice samples. Among the examined materials, sol-gel C coated titania-based FPSE membranes showed the highest extraction efficiency.

Investigating the applicability of polar fabric phase sorptive extraction for the HPLC quantitation of salivary vitamin B following administration of sublingual tablets and oral sprays.

In this study, a simple and rapid fabric phase sorptive extraction (FPSE) protocol combined with high performance liquid chromatography-ultraviolet detection (HPLC-UV) was developed for the monitoring of salivary vitamin B levels. Different sol-gel coated cellulose and polyester membranes were evaluated and sol-gel Carbowax 20 M coated polyester membranes were chosen for the selective extraction of the target analyte from saliva samples. Face-centered central composite design (FC-CCD) was employed for the investigation and optimization of sample volume, extraction time and stirring rate, while the other experimental factors were investigated using the classical one-factor-at-a- time" (OFAT) method.

LC-MS/MS Application in Pharmacotoxicological Field: Current State and New Applications.

Nowadays, it is vital to have new, complete, and rapid methods to screen and follow pharmacotoxicological and forensic cases. In this context, an important role is undoubtedly played by liquid chromatography-tandem mass spectrometry (LC-MS/MS) thanks to its advanced features. This instrument configuration can offer comprehensive and complete analysis and is a very potent analytical tool in the hands of analysts for the correct identification and quantification of analytes.

Sol-Gel Graphene Oxide-Coated Fabric Disks as Sorbents for the Automatic Sequential-Injection Column Preconcentration for Toxic Metal Determination in Distilled Spirit Drinks.

Sol-gel graphene oxide-coated polyester fabric platforms were synthesized and used for the on-line sequential injection fabric disk sorptive extraction (SI-FDSE) of toxic (i.e., Cd(II), Cu(II) and Pb(II)) metals in different distilled spirit drinks prior to their determination by electrothermal atomic absorption spectrometry (ETAAS).

Investigating the Use of SARS-CoV-2 (COVID-19) Odor Expression as a Non-Invasive Diagnostic Tool-Pilot Study.

Since the beginning of the COVID-19 pandemic, there has been enormous interest in the development of measures that would allow for the swift detection of the disease. The rapid screening and preliminary diagnosis of SARS-CoV-2 infection allow for the instant identification of possibly infected individuals and the subsequent mitigation of the disease spread. Herein, the detection of SARS-CoV-2-infected individuals was explored using noninvasive sampling and low-preparatory-work analytical instrumentation.

Hydrophilic interaction liquid chromatography-electrospray ionization mass spectrometry combined with fabric phase sorptive extraction for therapeutic drug monitoring of pioglitazone, repaglinide, and nateglinide in human plasma.

Polypharmacy in type 2 diabetes is an issue of major concern as the prescription of multiple medi-cations for the management of diabetes-associated comorbidities can lead to drug-to-drug interactions, which can pose serious risks to patients' health. Within this context, the development of bioanalytical methods for monitoring the therapeutic levels of antidiabetic drugs is notably useful to ensure patients' safety. In the present work, a liquid chromatography-mass spectrometry method for the quantitation of pioglitazone, repaglinide, and nateglinide in human plasma is described.

The Use of Biological Sensors and Instrumental Analysis to Discriminate COVID-19 Odor Signatures.

The spread of SARS-CoV-2, which causes the disease COVID-19, is difficult to control as some positive individuals, capable of transmitting the disease, can be asymptomatic. Thus, it remains critical to generate noninvasive, inexpensive COVID-19 screening systems. Two such methods include detection canines and analytical instrumentation, both of which detect volatile organic compounds associated with SARS-CoV-2.

Fabric phase sorptive extraction combined with high performance liquid chromatography for the determination of favipiravir in human plasma and breast milk.

A fast procedure obtained by the combination of fabric phase extraction (FPSE) with high performance liquid chromatography (HPLC) has been developed and validated for the quantification of favipiravir (FVP) in human plasma and breast milk. A sol-gel polycaprolactone-block-polydimethylsiloxane-block-polycaprolactone (sol-gel PCAP-PDMS-PCAP) coated on 100% cellose cotton fabric was selected as the most efficient membrane for FPSE in human plasma and breast milk samples. HPLC-UV analysis were performed using a RP C18 column under isocratic conditions.

Dual Lab-in-Syringe Flow-Batch Platform for Automatic Fabric Disk Sorptive Extraction/Back-extraction as a Front End to Inductively Coupled Plasma Atomic Emission Spectrometry.

A novel dual lab-in-syringe flow-batch (D-LIS-FB) platform for automatic fabric-disk-in-syringe sorptive extraction followed by oxidative back-extraction as a front end to inductively coupled plasma atomic emission spectrometry (ICP-AES) is presented for the first time. Sol-gel poly(caprolactone)-poly(dimethylsiloxane)-poly(caprolactone)-coated polyester fabric disks were packed at the top of the glass barrel of a microsyringe pump as an alternative to column preconcentration. Herein lie multiple significant advantages including effectiveness, compactness, lower back-pressure, and lower time of analysis.

Designing an "all-in-one" microextraction capsule device for the liquid chromatographic-fluorescence determination of doxorubicin and its metabolites in rat plasma.

In this study, an "all-in-one" microextraction device was designed and fabricated for the extraction of doxorubicin and its two metabolites from rat plasma prior to their determination by high performance liquid chromatography coupled to fluorescence detector. A sol-gel-based sorbent was synthesized in situ and incorporated within two conjoined porous polypropylene tubes together with a cylindrical magnetic bar in order to avoid the need of an external stirring bar. Among other sorbents investigated, the moderately polar sol-gel poly(tetrahydrofuran) was found to be advantageous due to its high affinity toward the target analytes.

An automatic on-line sol-gel pyridylethylthiopropyl functionalized silica-based sorbent extraction system coupled to flame atomic absorption spectrometry for lead and copper determination in beer samples.

A novel sol-gel pyridylethylthiopropyl functionalized silica-based sorbent was synthesized and utilized in an on-line column preconcentration system coupled with flame atomic absorption spectrometry for metal determination. The developed platform was used for the determination of Pb(II) and Cu(II) in beer samples, since there are limited automatic methods for routine analysis of alcoholic beverage. For a preconcentration time of 60 s, the calculated enhancement factors were 96 for Cu(II) and 130 for Pb(II).

Magnet integrated fabric phase sorptive extraction as a stand-alone extraction device for the monitoring of benzoyl urea insecticides in water samples by HPLC-DAD.

Benzoyl urea insecticides are a class of pesticides used in agriculture for the inhibition of chitin synthesis in pests. These compounds are persistent in environmental samples, and thus their monitoring is necessary to avoid detrimental effects to human health and the environment. Magnet integrated fabric phase sorptive extraction (MI-FPSE) is a recently introduced sample preparation technique that combines sample stirring and analyte extraction into one stand-alone device.