scholarly journals Beta-Cyclodextrin-Decorated Magnetic Activated Carbon as a Sorbent for Extraction and Enrichment of Steroid Hormones (Estrone, β-Estradiol, Hydrocortisone and Progesterone) for Liquid Chromatographic Analysis

Molecules ◽  
2021 ◽  
Vol 27 (1) ◽  
pp. 248
Author(s):  
Anele Mpupa ◽  
Azile Nqombolo ◽  
Boris Mizaikoff ◽  
Philiswa Nosizo Nomngongo
Keyword(s):  
Electron Microscopy ◽  
Activated Carbon ◽  
High Performance ◽  
Solid Phase ◽  
Extraction Procedure ◽  
Carbon Adsorbent ◽  
Analytical Techniques ◽  
Array Detector ◽  
Magnetic Activated Carbon ◽  
Wastewater Samples

A β-cyclodextrin-decorated magnetic activated carbon adsorbent was prepared and characterized using various analytical techniques (X-ray diffraction (XRD), scanning electron microscopy–electron diffraction spectroscopy (SEM-EDS) and transmission electron microscopy (TEM)), and the adsorbent was used in the development of a magnetic solid-phase microextraction (MSPE) method for the preconcentration of estrone, β-estradiol, hydrocortisone and progesterone in wastewater and river water samples. This method was optimized using the central composite design in order to determine the experimental parameters affecting the extraction procedure. The quantification of hormones was achieved using high-performance liquid chromatography equipped with a photodiode array detector (HPLC-DAD). Under optimum conditions, the linearity ranged from 0.04 to 300 µg L−1 with a correlation of determinations of 0.9969–0.9991. The limits of detection and quantification were between 0.01–0.03 and 0.033–0.1 µg L−1, with intraday and interday precisions at 1.1–3.4 and 3.2–4.2. The equilibrium data were best described by the Langmuir isotherm model, and high adsorption capacities (217–294 mg g−1) were obtained. The developed procedure demonstrated high potential as an effective technique for use in wastewater samples without significant interferences, and the adsorbent could be reused up to eight times.

scholarly journals Analysis of Intact Glycosidic Aroma Precursors in Grapes by High-Performance Liquid Chromatography with a Diode Array Detector

Foods ◽  
2021 ◽  
Vol 10 (1) ◽  
pp. 191
Author(s):  
Cristina Cebrián-Tarancón ◽  
José Oliva ◽  
Miguel Ángel Cámara ◽  
Gonzalo L. Alonso ◽  
M. Rosario Salinas
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Solid Phase ◽  
Analytical Techniques ◽  
Array Detector ◽  
Diode Array ◽  
Diode Array Detector ◽  
Analytical Technique ◽  
Aroma Precursors

Nowadays, the techniques for the analysis of glycosidic precursors in grapes involve changes in the glycoside structure or it is necessary the use of very expensive analytical techniques. In this study, we describe for the first time an approach to analyse intact glycosidic aroma precursors in grapes by high-performance liquid chromatography with a diode array detector (HPLC-DAD), a simple and cheap analytical technique that could be used in wineries. Briefly, the skin of Muscat of Alexandria grapes was extracted using a microwave and purified using solid-phase extraction combining Oasis MCX and LiChrolut EN cartridges. In total, 20 compounds were selected by HPLC-DAD at 195 nm and taking as a reference the spectrum of phenyl β-D-glucopyranoside, whose DAD spectrum showed a first shoulder from 190 to 230 nm and a second around 200–360 nm. After that, these glycosidic compounds were identified by High-performance liquid chromatography–quadrupole time-of-flight mass spectrometry (HPLC-qTOF-MS). Disaccharides hexose pentose were the most abundant group observed with respect to the sugars and monoterpendiols the main aglycones found.

scholarly journals Amine-functionalized magnetic activated carbon as an adsorbent for preconcentration and determination of acidic drugs in environmental water samples using HPLC-DAD

2020 ◽  
Vol 18 (1) ◽  
pp. 1218-1229 ◽  
Author(s):  
Mpingana Ndilimeke Akawa ◽  
Kgogobi Mogolodi Dimpe ◽  
Philiswa Nosizo Nomngongo
Keyword(s):  
Activated Carbon ◽  
River Water ◽  
Water Samples ◽  
High Performance ◽  
Solid Phase ◽  
Magnetic Solid Phase Extraction ◽  
Array Detector ◽  
Acidic Drugs ◽  
Relative Standard

AbstractIn the present study, a convenient and highly effective method was developed for the quantification of acidic drugs in wastewater and river water samples. Ultrasonic-assisted magnetic solid phase extraction employing magnetic waste tyre-based activated carbon nanocomposite functionalized with [3-(2-aminoethylamino)propyl]trimethoxysilane as a cost-effective and efficient adsorbent was used for the extraction and preconcentration of acidic drugs (naproxen [NAP], ketoprofen (KET) and diclofenac [DIC]). The quantification of target analytes was achieved by high‐performance liquid chromatography with diode array detector. Under optimum conditions, the detection limit, quantification limit and relative standard deviation obtained for the analytes of interest ranged from 0.38 to 0.76, 1.26 to 2.54 µg L−1 and 2.02 to 4.06%, respectively. The applicability of the developed method was assessed by the spike recovery tests and the relative recoveries proved that the method is reliable for the determination of acidic drugs in wastewater. Thereafter, the method was applied successfully for the determination of NAP, KET and DIC in river water, influent and effluent wastewater.

scholarly journals Separation of aniline from water and wastewater samples based on activated carbon nanoparticles and dispersive solid phase extraction procedure

2020 ◽  
Vol 3 (04) ◽  
pp. 72-84
Author(s):  
Saeed Fakhraie ◽  
Morteza Mehdipour Rabouri ◽  
Ahmad Salarifar
Keyword(s):  
Ionic Liquid ◽  
Activated Carbon ◽  
Solid Phase Extraction ◽  
Solid Phase ◽  
Extraction Procedure ◽  
Phase Extraction ◽  
Carboxylic Groups ◽  
Solid Phase Extraction Procedure ◽  
Water And Wastewater ◽  
Wastewater Samples

The water, wastewater and air are the main sources of aniline in environment. Aniline has a toxic effect in the human body and environment and so, must be determined by novel techniques. In this study, the activated carbon with microwave heating methods (MHM-ACNPs) were used for extraction aniline from waters by dispersive ionic liquid solid phase extraction procedure (D-IL-SPE) and compared to the activated carbon (AC). For this purpose, the mixture of acetone, ionic liquid and 30 mg of MHM-ACNPs/AC added to 100 mL of water samples at pH=8. After sonication for 10 min, the benzene ring in aniline as electron acceptor was chemically adsorbed on carboxylic groups of MHM-ACNPs as electron donors (MHM-ACNPs-COO─……C6H5-NH2) and then, the adsorbent was collected by IL phase in bottom of conical centrifuging tube. Finally, the aniline was released from MHM-ACNPs in remained solution by changing pH and the concentration of aniline determined by GC-FID.

scholarly journals Simultaneous Determination of Seven Antibiotics and Five of Their Metabolites in Municipal Wastewater and Evaluation of Their Stability under Laboratory Conditions

2021 ◽  
Vol 18 (20) ◽  
pp. 10640
Author(s):  
Sheng Han ◽  
Xinyue Li ◽  
Hongmei Huang ◽  
Ting Wang ◽  
Zhenglu Wang ◽  
...  
Keyword(s):  
Public Health ◽  
High Performance ◽  
Municipal Wastewater ◽  
Therapeutic Potential ◽  
Solid Phase ◽  
Human Pathogens ◽  
Removal Rates ◽  
Liquid Chromatography Tandem Mass ◽  
Antibiotics Use ◽  
Wastewater Samples

The selection and spread of antibiotic resistance poses risks to public health by reducing the therapeutic potential of antibiotics against human pathogens. Wastewater-based epidemiology (WBE) is potentially the most reliable approach to estimate antibiotics use. Previous WBE studies used parent antibiotics as biomarkers, which may lead to overestimation since parent antibiotics may be directly disposed of. Using metabolites as biomarkers can avoid this drawback. This study developed a simultaneous solid-phase extraction coupled with ultra-high-performance liquid chromatography tandem mass spectrometry method for analyzing 12 antibiotics and human metabolites in wastewater to help assess health risk. Optimum conditions were achieved using a PEP cartridge at pH 3.0. The extraction efficiencies were 73.3~95.4% in influent and 72.0~102.7% in effluent for most of the target analytes. Method detection limit ranged from 0.1 to 1.5 ng/L for influent wastewater and 0.03 to 0.7 ng/L for effluent wastewater. A stability experiment showed that sulfonamide parents and their metabolites were stable at 4 °C, −20 °C and −80 °C, while macrolides metabolites were more stable than their corresponding parents at 4 °C and −20 °C. Finally, the method was applied to measure these analytes in wastewater samples collected from three Beijing WWTPs and to derive apparent removal rates. All metabolites were detected in wastewater samples with concentrations ranging from 1.2 to 772.2 ng/L in influent, from <MDL to 235.6 ng/L in effluent. The apparent removal rates of five metabolites were above 72.6%. These results set a solid foundation for applying WBE to evaluate antibiotics use and its public health effects.

scholarly journals Characterization of Volatile and Flavonoid Composition of Different Cuts of Dried Onion (Allium cepa L.) by HS-SPME-GC-MS, HS-SPME-GC×GC-TOF and HPLC-DAD

Molecules ◽  
2020 ◽  
Vol 25 (2) ◽  
pp. 408 ◽  
Author(s):  
Lorenzo Cecchi ◽  
Francesca Ieri ◽  
Pamela Vignolini ◽  
Nadia Mulinacci ◽  
Annalisa Romani
Keyword(s):  
Gas Chromatography ◽  
High Performance ◽  
Solid Phase ◽  
Array Detector ◽  
Volatile Fraction ◽  
Solid Phase Micro Extraction ◽  
Food Ingredient ◽  
Head Space ◽  
Dipropyl Disulfide ◽  
Allium Cepa L

Onion is widely used worldwide in various forms for both food and medicinal applications, thanks to its high content of phytonutrients, such as flavonoids and volatile sulfur compounds. Fresh onion is very perishable and drying is widely applied for extending shelf-life, thus obtaining a very easy-to-use functional food ingredient. The flavonoid and volatile fractions of different onion cuts (flakes, rings) prepared through different drying cycles in a static oven, were characterized by high-performance liquid chromatography with a diode-array detector HPLC-DAD, Head Space-Solid Phase Micro Extraction followed by Gas Chromatography coupled with Mass Spectrometry (HS-SPME-GC-MS) and Head-Space Solid Phase Micro Extraction followed by comprehensive two-dimensional Gas-Chromatography (HS-SPME-GC×GC-TOF). Onion flakes showed a significantly higher flavonoid content (3.56 mg g−1) than onion rings (2.04 mg g−1). Onion flakes showed greater amount of volatile organic compounds (VOCs) (127.26 mg g−1) than onion rings (42.79 mg g−1), with different relative amounts of di- and trisulfides—disulfides largely predominate the volatile fraction (amounts over 60% on the total volatile content), followed by trisulfides and dipropyl disulfide and dipropyl trisulfide were the most abundant VOCs. HS-SPME-GC×GC-TOF allowed for the detection of the presence of allylthiol, diethanol sulfide, 4,6-diethyl1,2,3,5-tetrathiolane, not detected by HS-SPME-GC-MS, and provided a fast and direct visualization and comparison of different samples. These results highlight different nutraceutical properties of dried onion samples processed otherwise, only differing in shape and size, thus pointing out potentially different uses as functional ingredients.

scholarly journals Razvoj SPE-HPLC-DAD metode za određivanje florfenikola i florfenikol amina u cerebrospinalnoj tekućini svinja

2020 ◽  
Vol 51 (2) ◽  
pp. 129-138
Author(s):  
Ksenija Šandor ◽  
Svjetlana Terzić ◽  
Anja Vujnović ◽  
Eleonora Perak Junaković ◽  
Irena Žarković ◽  
...  
Keyword(s):  
Cerebrospinal Fluid ◽  
High Performance ◽  
Solid Phase ◽  
Biological Fluids ◽  
Experimental Period ◽  
Intramuscular Administration ◽  
Array Detector ◽  
Control Group ◽  
Pharmacokinetic Studies ◽  
Experimental Conditions

A study of florfenicol (FF) and its metabo- lite florfenicol amine (FFA) in pig cerebrospinal fluid was conducted following repeated intramuscular administration of the original (reference) and a generic veterinary medicinal product (VMP) under the same experimental conditions (20 mg FF/kg body weight, 48-hour interval). Both VMPs are solutions for injection containing FF as an active substance in the concentration of 300 mg/mL and have been authorized in Croatia for use in cattle and pigs. In this study, clinically healthy pigs were randomly divided into three groups. The first group was treated with the reference VMP, the second with the generic VMP, while the third served as the control group. Animals were sacrificed at 216, 288 and 384 hours after the first drug administration. Cerebrospinal fluid samples were analysed by the optimized and validated high-performance liquid chromatography-diode array detector method (HPLC-DAD). The solid-phase extraction (SPE) technique was chosen for sample preparation. The HPLC-DAD method provides good linearity over the concentration range of 0.05 to 5.00 μg/mL for FF and FFA. Limits of detection were 0.0023 μg/mL for FF and 0.0100 μg/mL for FFA. Extraction recoveries of FF were from 86.6% to 111.8%, and of FFA from 91.7% to 98.8%. The SPE-HPLC-DAD method has been demonstrated to be a selective, sensitive and suitable analytical method for the determination of FF and FFA in cerebrospinal fluid. The present study was based on a preliminary study that quantified FF in pig plasma at 216 hours after the first application of reference or generic VMP. However, FF and FFA were not detected in any of the cerebrospinal fluid samples during the experimental period. According to the nature of biological fluids, the SPE-HPLC-DAD method can be suitable for further pharmacokinetic studies of FF in pig plasma and serum after intramuscular administration of VMPs.

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