Solid-phase microextraction (SPME) is a sample preparation technique with many applications that is being continuously developed. In this technique, the type of fiber coating plays a crucial role for extraction efficiency. Currently available commercial coatings have certain drawbacks that have been overcome by the development of new coatings based on novel materials; these have improved the efficiency of extraction, selectivity and stability of commercial coatings. Pharmaceutical and personal care products (PPCPs) are one of the most important groups of emerging contaminants; however, some studies suggest that these compounds can cause adverse health effects. No official monitoring protocols for these compounds are currently available, so the establishment of analytical methods that allow their determination in environmental samples is required. The complexity of environmental samples together with the low concentration levels of these compounds makes necessary the use of sample preparation techniques capable of removing interferences, as well as preconcentrated analytes, and SPME is a very promising alternative to achieve this. This review describes the recent developments in SPME with classical and novel coatings and its applications for PPCP determination in environmental samples.
Abstract. A novel coating for solid-phase microextraction (SPME) fibers was manufactured by using a mixture of 1-decyl-3methylimidazolium tetrafluoroborate ionic liquid and a commercial adhesive deposited on an etched stainless-steel support. The new coating was characterized by applying optical and electron microscopy, infrared spectroscopy and its extraction capacity was also evaluated. The extraction capacity was tested using as model analytes some pharmaceutical and personal care products (PPCPs) with different hydrophilicities. The potential use of the new fiber was evaluated through direct-immersion mode extractions and showed extraction capacity toward methylparaben, propylparaben, naproxen, diclofenac and benzophenone-3. Experimental design tools were used to study and optimize the variables that affect the extraction and desorption processes of the SPME by direct immersion. The analytical performance of proposed method was investigated under SPME procedure´s optimal conditions, coupled to a high-performance liquid chromatography-diode array detector (HPLC-DAD) method, which was developed and validated for analysis of the target PPCPs. The method of SPME by direct immersion was linear, precise and accurate. Detection and quantification limits of 0.023 to 0.093 μg mL-1 and 0.118 to 0.279 μg mL-1 were obtained, respectively. By the use of the developed method, tap water samples were analyzed and recoveries from 3.39 to 183.29 % were found. The new fiber presented an adequate stability and good extraction reproducibility (<15 % RSD). As a final point, this device is of easy and quick preparation, inexpensive, and suitable for extraction of some PPCPs. Resumen. Se fabricó un nuevo recubrimiento para fibras de microextracción en fase sólida (SPME) utilizando una mezcla del líquido iónico tetrafluoroborato de 1-decil-3metilimidazolio y un adhesivo comercial depositada sobre un soporte de acero inoxidable grabado. El nuevo recubrimiento se caracterizó mediante la aplicación de microscopía óptica y electrónica, espectroscopía de infrarrojo y también se evaluó su capacidad de extracción. La capacidad de extracción se probó utilizando como analitos modelo algunos productos farmacéuticos y de cuidado personal (PPCPs) con diferentes hidrofilicidades. El uso potencial de la nueva fibra se evaluó mediante extracciones en modo de inmersión directa y mostró capacidad de extracción hacia metilparabeno, propilparabeno, naproxeno, diclofenaco y benzofenona-3. Se utilizaron herramientas del diseño experimental para estudiar y optimizar las variables que afectan los procesos de extracción y desorción de la SPME por inmersión directa. El rendimiento analítico del método propuesto se investigó en las condiciones óptimas del procedimiento de SPME, acoplado a un método de cromatografía líquida de alto rendimiento con detector de arreglo de diodos (HPLC-DAD), que fue desarrollado y validado para el análisis de los PPCPs objetivo. El método de SPME por inmersión directa fue lineal, preciso y exacto. Se obtuvieron límites de detección y cuantificación de 0.023 a 0.093 μg mL-1 y 0.118 a 0.279 μg mL-1, respectivamente. Mediante el uso del método desarrollado, se analizaron muestras de agua del grifo y se encontraron recuperaciones de 3.39 a 183.29 %. La nueva fibra presentó una adecuada estabilidad y buena reproducibilidad de extracción (<15 % RSD). Como punto final, este dispositivo es de fácil y rápida preparación, económico y adecuado para la extracción de algunos PPCPs.
The analysis of phenolic acids (PAs) is of great importance, because they are frequently present in natural products and their derivatives, and these compounds also have multiple beneficial effects to human health. This work is focusing on the separation of seven PAs (caffeic acid, coumaric acid, gallic acid, ferulic acid, protocatechuic acid, sinapic acid, and syringic acid), in a reversed-phase liquid chromatographic (RP-HPLC) isocratic method using a hydrophilic deep eutectic solvent (DES) as a mobile phase additive. The analysis was carried out with a diode array detector. The used DES was composed by choline chloride and glycerol, and it was characterized by infrared spectroscopy. The combination of choline chloride:glycerol (1:4) added at 0.25% to mobile phase composed of 0.15% formic acid aqueous solution and methanol (80:20), showed the best separation for target analytes. The new proposed method was validated, and results indicated that the proposed method is linear, selective for almost all analytes, provided high sensitivity with limit of detection ranges from 0.009 to 0.023 mg mL−1, and has satisfactory precision and accuracy, with values of relative standard deviation of 0.24–2.65% and recoveries of 97.97–109%, respectively. Additionally, this method was successfully applied to simultaneous determination of phenolic acids in three kinds of samples of powder to prepare lemon flavour drink enriched with black tea extract.
Recently, pharmaceutical and personal care products (PPCPs) have received considerable attention because of their increasing use. Analysis of PPCPs presents a significant analytical challenge, with high-performance liquid chromatography (HPLC) in reversed-phase mode, as the most widely used analytical technique. To facilitate the optimization of the procedures that are applied in the early stages of sample preparation, a simple and fast HPLC method is proposed in this work for the separation of some PPCPs with a wide range of hydrophilicity. Two columns were evaluated (Atlantis dC18 and Discovery HS F5); as for mobile phases: a formate buffer (40 mmol L−1, pH 4) and methanol were tested in a gradient mode. The fluorinated column allowed better separation in a shorter time and better resolution for all analytes (Rs > 1). The proposed method delivered good performance for the tracing of PPCPs and is a suitable alternative to traditional C18-based HPLC methods.
Currently, sample preparation is the most laborious part of the analytical process, requiring the most time and being susceptible to the most errors. In this context, numerous investigations have focused on the miniaturization of these techniques to reduce work time, costs, and errors. In this regard, microextraction by packed sorbent (MEPS) is a simple, fast, and robust sample preparation technique suitable for easy automation in several analytical systems and is applied to a wide variety of samples. Antibiotics are among the most commonly used drugs; however, their extensive and inappropriate use has garnered significant attention in the environment, human health, and food safety. This brief review is intended to provide an overview of recently reported antibiotic extraction methods based on MEPS, with a special interest in those applied to the analysis of biological, environmental, and food samples. In addition, the sample pretreatment step before extraction by the MEPS device was highlighted, as was the description of the sample-related steps within the MEPS procedure, such as extraction, washing, and elution.
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