RESUMEN
The analysis of dietary supplements is far less regulated than pharmaceuticals, leading to potential quality issues. Considering their positive effect, many athletes consume supplements containing L-histidine and ß-alanine. A new microfluidic method for the determination of L-histidine and ß-alanine in dietary supplement formulations has been developed. For the first time, capacitively coupled contactless conductivity detection was employed for the microchip electrophoresis of amino acids in real samples. A linear relationship between detector response and concentration was observed in the range of 10-100 µmol L-1 for L-histidine (R2 = 0.9968) and ß-alanine (R2 = 0.9954), while achieved limits of detection (3 × S/N ratio) were 4.2 µmol L-1 and 5.2 µmol L-1, respectively. The accuracy of the method was confirmed using recovery experiments as well as CE-UV-VIS and HPLC-UV-VIS techniques. The developed method allows unambiguous identification of amino acids in native form without chemical derivatization and with the possibility of simultaneous analysis of amino acids with metal cations.
Asunto(s)
Suplementos Dietéticos , Conductividad Eléctrica , Electroforesis por Microchip , Histidina , beta-Alanina , Electroforesis por Microchip/métodos , Suplementos Dietéticos/análisis , beta-Alanina/análisis , beta-Alanina/química , Histidina/análisis , Histidina/química , Límite de Detección , Tecnología Química Verde/métodos , Vidrio/químicaRESUMEN
The health supplement industry is one of the fastest growing industries in the world, but there is a lack of suitable analytical methods for the determination of active compounds in health supplements such as peptides. The present work describes an implementation of contactless conductivity detection on microchip technology as a new strategy for the electrophoretic determination of L-carnosine in complex health supplement formulations without pre-concentration and derivatization steps. The best results were obtained in the case of +1.00 kV applied for 20 s for injection and +2.75 kV applied for 260 s for the separation step. Under the selected conditions, a linear detector response of 5 × 10-6 to 5 × 10-5 M was achieved. L-carnosine retention time was 61 s. The excellent reproducibility of both migration time and detector response confirmed the high precision of the method. The applicability of the method was demonstrated by the determination of L-carnosine in three different samples of health supplements. The recoveries ranged from 91 to 105%. Subsequent analysis of the samples by CE-UV-VIS and HPLC-DAD confirmed the accuracy of the obtained results.
Asunto(s)
Carnosina , Electroforesis por Microchip , Electroforesis por Microchip/métodos , Reproducibilidad de los Resultados , Inyecciones , Conductividad Eléctrica , Dispositivos Laboratorio en un ChipRESUMEN
Thiabendazole (TBZ) is a fungicide and anthelmintic drug commonly found in food products. Due to its toxicity and potential carcinogenicity, its determination in various samples is important for public health. Different analytical methods can be used to determine the presence and concentration of TBZ in samples. Liquid chromatography (LC) and its subtypes, high-performance liquid chromatography (HPLC) and ultra-high-performance liquid chromatography (UHPLC), are the most commonly used methods for TBZ determination representing 19%, 18%, and 18% of the described methods, respectively. Surface-enhanced Raman spectroscopy (SERS) and fluorimetry are two more methods widely used for TBZ determination, representing 13% and 12% of the described methods, respectively. In this review, a number of methods for TBZ determination are described, but due to their limitations, there is a high potential for the further improvement and development of each method in order to obtain a simple, precise, and accurate method that can be used for routine analysis.
Asunto(s)
Fungicidas Industriales , Tiabendazol , Tiabendazol/análisis , Cromatografía Líquida de Alta Presión/métodos , Cromatografía Liquida/métodos , Fungicidas Industriales/análisis , FluorometríaRESUMEN
Promethazine hydrochloride (PM) is a widely used drug so its determination is important. Solid-contact potentiometric sensors could be an appropriate solution for that purpose due to their analytical properties. The aim of this research was to develop solid-contact sensor for potentiometric determination of PM. It had a liquid membrane containing hybrid sensing material based on functionalized carbon nanomaterials and PM ions. The membrane composition for the new PM sensor was optimized by varying different membrane plasticizers and the content of the sensing material. The plasticizer was selected based on calculations of Hansen solubility parameters (HSP) and experimental data. The best analytical performances were obtained using a sensor with 2-nitrophenyl phenyl ether (NPPE) as the plasticizer and 4% of the sensing material. It had a Nernstian slope (59.4 mV/decade of activity), a wide working range (6.2 × 10-7 M-5.0 × 10-3 M), a low limit of detection (1.5 × 10-7 M), fast response time (6 s), low signal drift (-1.2 mV/h), and good selectivity. The working pH range of the sensor was between 2 and 7. The new PM sensor was successfully used for accurate PM determination in a pure aqueous PM solution and pharmaceutical products. For that purpose, the Gran method and potentiometric titration were used.
RESUMEN
A new sensor for direct potentiometric determination of thiabendazole (TBZ) was prepared. The ionic pair of TBZ cation and the 5-sulfosalicylate anion was used as the new sensor material incorporated in liquid type of ion-selective electrode membrane for TBZ determination. For optimization of the membrane of the sensor for TBZ determination, six different plasticizers and the content of the sensor material in the membrane were varied. The chosen sensor with dibutyl sebacate (DS) as plasticizer and 1% of sensor material in the membrane was characterized with Nernstian response towards TBZ (62.2 mV/decade of activity), a wide working range (8.6â10-7-1.0â10-3 M), and a low limit of detection (3.2·10-7 M). Also, it proved to be an accurate and reliable sensor for TBZ determination in pure and real samples (peel of oranges, lemons and bananas) where it was determined using direct potentiometry and Gran method.
Asunto(s)
Citrus , Tiabendazol , Frutas , Plastificantes , PotenciometríaRESUMEN
Direct potentiometric measurements using solid-state sensors have a great potential for thiabendazole (TBZ) determination, considering simplicity, accuracy, and low cost. Modifying the sensing material of the sensor with multi-walled carbon nanotubes (MWCNTs) leads to improved analytical properties of the sensor. In this study, a new potentiometric solid-state sensor for TBZ determination, based on MWCNTs modified with a sulfate group, and TBZ ion as sensing material was developed. The sensor exhibited a Nernstian response for TBZ (60.4 mV/decade of activity) in a working range between 8.6 × 10-7 and 1.0 × 10-3 M. The detection limit for TBZ was 6.2 × 10-7 M. The response time of the sensor for TBZ was 8 s, and its signal drift was only 1.7 mV/h. The new sensor is applicable for direct potentiometric determination of TBZ in complex real samples, such as fruit peel. The accuracy of TBZ determination is confirmed using the standard addition method.
Asunto(s)
Nanotubos de Carbono , Materiales Inteligentes , Electrodos , Potenciometría , TiabendazolRESUMEN
A new solid-state potentiometric sensor for anionic surfactants (AnS) determination was prepared. The sensor material in the liquid membrane was made of multi-walled carbon nanotubes (MWCNTs) chemically functionalized with a quaternary ammonium group and tetraphenylborate (TPB) anion (MWCNT-N+(CH3)3TPB-). The response of the MWCNT-N+(CH3)3TPB- sensor was Nernstian (59.3 mV/decade of activity) for both AnS investigated (sodium dodecyl sulfate (NaDDS) and sodium dodecylbenzenesulfonate (NaDBS)). The limits of detection were 2.0 â 10-7 and 1.5 â 10-7 for NaDDS and NaDBS, respectively, and the average response time was only 5 s. The new MWCNT-N+(CH3)3TPB- sensor was very selective for NaDDS compared to anions usually contained in commercial products and is not affected by nonionic surfactants that can also be present in these products. It was tested to determine AnS concertation by the potentiometric titration method in a pH range between 3 and 12 and successfully applied for its determination in three-component mixtures and real systems.