Water, renowned for its sustainability and minimal toxicity, is an ideal candidate for environmentally friendly solvent-based microextraction. However, its potential as an extractant solvent in miniaturized sample preparation remains largely unexplored. This paper pioneers using water as the extraction solvent in headspace single-drop microextraction (HS-SDME) for N-nitrosamines from losartan tablets.
View Article and Find Full Text PDFPreparative liquid chromatography is a technique for separating complex samples or isolating pure compounds from complex extracts. It involves eluting samples through a packed column and selectively collecting or isolating the separated bands in a sequence of fractions. Depending on the column length and the sample complexity, a large number of fractions may be obtained, making fraction collection a laborious and time-consuming process.
View Article and Find Full Text PDFNano-liquid chromatography (nanoLC) is gaining significant attention as a primary analytical technique across various scientific domains. Unlike conventional high-performance LC, nanoLC utilizes columns with inner diameters (i.ds.
View Article and Find Full Text PDFAn automated microextraction by packed sorbent followed by liquid chromatography-tandem mass spectrometry (MEPS-LC-MS/MS) method was developed for the determination of four endocrine disruptors-parabens, benzophenones, and synthetic phenolic antioxidants-in wastewater samples. The method utilizes a lab-made repackable MEPS device and a multi-syringe robotic platform that provides flexibility to test small quantities (2 mg) of multiple extraction phases and enables high-throughput capabilities for efficient method development. The overall performance of the MEPS procedure, including the investigation of influencing variables and the optimization of operational parameters for the robotic platform, was comprehensively studied through univariate and multivariate experiments.
View Article and Find Full Text PDFThis work presents a study on the application of wall open tubular column (WCOT) in liquid chromatography coupled with tandem mass spectrometry. Each process step reports the column preparation method in detail, subdivided into column pretreatment, silanization, stationary phase coating, and immobilization. Then, an evaluation of the parameters that can affect the efficiency of these columns was made.
View Article and Find Full Text PDFThe development of a fast, cost-effective, and efficient microextraction by packed sorbent setup was achieved by combining affordable laboratory-repackable devices of microextraction with a high-throughput cartesian robot. This setup was evaluated for the development of an analytical method to determine N-nitrosamines in losartan tablets. N-nitrosamines pose a significant concern in the pharmaceutical market due to their carcinogenic risk, necessitating their control and quantification in pharmaceutical products.
View Article and Find Full Text PDFThe present paper describes an original method for the online preconcentration and analysis of ring-substituted amphetamines in urine samples, used on the integration of robot-assisted hollow fiber liquid-phase microextraction (HF-LPME), high-performance liquid chromatography (HPLC), and fluorescence detection (FLD). A lab-made autosampler, actuating a 100-μL syringe and equipped with a three-way solenoid microvalve, allowed the acceptor phase to flow through and be withdrawn from the lumen fiber, enabling the automated online transference of the enriched acceptor phase for chromatographic analysis, through a six-port switching valve. The developed online HF-LPME-LC/FLD method demonstrated high analytical throughput and confidence, facilitating the efficient extraction and determination of the target analytes, with minimal solvent consumption and sample manipulation, in a straightforward way.
View Article and Find Full Text PDFA high-throughput and innovative setup has been developed to automate the online integration of single drop microextraction (SDME), liquid chromatography (LC) and high-resolution mass spectrometry (QqToF). SDME and LC were online hyphenated for the first time. SDME was carried out by a lab-made cartesian robot actuating a 100 μL syringe, equipped with a three-way solenoid microvalve that allowed the online transference of the enriched extract to the chromatographic system, through a six-port switching valve.
View Article and Find Full Text PDFIn this work, the dispersive liquid-liquid microextraction technique based on the solidification of the organic phase (DLLME-SFO) has been automated for the first time. DLLME-SFO is automated by hyphenating a sequential injection analysis (SIA) system with a custom-made robotic phase separator. Automated in-syringe DLLME is followed by phase separation in a 3D printed device integrating a Peltier cell set, mounted on a multi-axis robotic arm.
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