Extraction Procedure For Separation Research Articles

A cleaner and eco-friendly approach to simultaneous extraction and characterization of essential oil and pectin from Assam lemon peel and its application for energy generation through TENG devices

Scientists have been working on developing a green bio-TENG for portable remote devices, including wearables in the biomedical sector. The process involves obtaining pectin, a green material with anti-microbial properties, as a Triboelectric material. This study focuses on the extraction of essential oil (EO) and pectin from Assam lemon peel simultaneously. A single-step strategy was optimized using a central composite design-based response surface approach. The extracted pectin yielded 4.19 ± 0.31 % and 11.53 ± 0.11 %, respectively. GC-MS analysis revealed 52 volatile components in the Assam lemon EOs, with limonin being 94.47 % and β-Bisabolene being 1.26 %. Only khusilal was found in the EOs, a rare discovery in the scientific domain. The extracted pectin showed good purity and antimicrobial properties. The in vitro activities of the citrus EO against microbial cultures revealed its activity in controlling and eradicating bacterial and fungal growth. Hydro distillation followed by enzyme treatment is a promising approach that combines two separate extraction procedures. The produced biopolymer showed the generation of electrical signals under minimal pressure and stretching and prevented microbial degeneration when applied to a nanogenerator.

Fabrication and characterization of SiO2@Fe3O4@nanodiamonds for vortex-assisted magnetic solid-phase extraction of lead in cigarette samples prior to FAAS detection

A novel, speed and accurate vortex-assisted magnetic solid-phase extraction procedure for separation–preconcentration and flame atomic absorption spectrometric determination of lead at trace levels has been proposed. Silica-coated magnetic nanodiamonds (SiO2@MNDs) as magnetic solid-phase extractor were fabricated and characterized by Fourier transform infrared spectroscopy, X-ray diffraction spectrometry and scanning electron microscopy. Pb(II) could be easily separated from the aqueous solution on the SiO2@MNDs by using a neodymium magnet. Analytical factors affecting the recoveries of Pb(II) such as pH, adsorbent amount, type and volume of eluent and sample volume were optimized. The preconcentration factor, the precision (RSD %, n = 5), the limit of detection and the limit of quantification were 5, 5.3%, 40.8 and 135 µg L−1, respectively. The effects of matrix ions have been investigated. The presented extraction method has been applied for the determination of lead in cigarette samples and Bush Branches and Leaves certified reference material. Quantitative recoveries changing from 94 to 106% were obtained for accuracy studies.

Selenium and selenium species in feeds and muscle tissue of Atlantic salmon

Selenium (Se) is an essential element for animals, including fish. Due to changes in feed composition for Atlantic salmon (Salmo salar), it may be necessary to supplement feeds with Se. In the present work, the transfer of Se and Se species from feed to muscle of Atlantic salmon fed Se supplemented diets was studied. Salmon were fed basal fish feed (0.35 mg Se/kg and 0.89 mg Se/kg feed), or feed supplemented either with selenised yeast or sodium selenite, at low (1–2 mg Se/kg feed) and high (15 mg Se/kg feed) levels, for 12 weeks. For the extraction of Se species from fish muscle, enzymatic cleavage with protease type XIV was applied. The extraction methods for Se species from fish feed were optimised, and two separate extraction procedures were applied, 1) enzymatic cleavage for organic Se supplemented feeds and 2) weak alkaline solvent for inorganic Se supplemented feeds, respectively. For selenium speciation analysis in feed and muscle tissue anion-exchange HPLC-ICP-MS for analysis of inorganic Se species and cation-exchange HPLC-ICP-MS for analysis of organic Se species, were applied. In addition, reversed phase HPLC-ICP-MS was applied for analysis of selenocysteine (SeCys) in selected muscle samples. The results demonstrated that supplemented Se (organic and inorganic) accumulated in muscle of Atlantic salmon, and a higher retention of Se was seen in the muscle of salmon fed organic Se diets. Selenomethionine (SeMet) was the major Se species in salmon fed basal diets and diets supplemented with organic Se, accounting for 91–118% of the total Se. In contrast, for muscle of salmon fed high inorganic Se diet, SeMet accounted for 30% of the total Se peaks detected. Several unidentified Se peaks were detected, in the fish fed high inorganic diet, and analysis showed indicated SeCys is a minor Se species present in this fish muscle tissue.

Rapid and sensitive screening and confirmation of thirty-four aminocarbonyl/carboxamide (NACA) and arylindole synthetic cannabinoid drugs in human whole blood.

We describe the development and validation of a method for the screening and confirmation of a range of chemically diverse synthetic cannabinoid drugs in human whole blood. The method targets the better known arylindole compounds as well as the emerging aminocarbonyl/ carboxamide (NACA) compounds. The approach consists of two separate extraction procedures designed to optimize recovery of each of these two classes, followed by analysis by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The most significant novel compounds added were AB-FUBINACA, ADBICA, 5 F-ADBICA, ADB-PINACA, ADB-FUBINACA, ADB-FUBINACA, 5 F-ADB-PINACA, 5 F-ADB-PINACA, AB-PINACA, AB-CHMINACA, and ADB-CHMINACA. A third procedure is described for the quantitative confirmation of those compounds for which deuterated internal standards permitted quantitative analysis, including JWH-018, JWH-122, JWH-081, JWH-210, AM-2201, XLR-11, and UR-144. The methods were successfully validated according to Scientific Working Group in Forensic Toxicology (SWGTOX) protocol for 34 compounds in common use in the United States in the period of 2014 and 2015, although other substances, unknown at the time may have been introduced to the market over the same time period. The method was determined to be free from carry-over between samples, and no interference was found from other common therapeutic abused or novel psychoactive drugs. The methods were applied to the analysis of 1142 blood samples from forensic investigations, including post-mortem examinations and driving impairment cases. The drugs most frequently detected were AB-CHMINACA (18.6%), ADB-CHMINACA (15%), XLR-11 (5.5%), AB-FUBINACA (4.5%), AB-PINACA (3.9%), and ADB-FUBINACA (2.3%). Copyright © 2016 John Wiley & Sons, Ltd.

Synthesis of 2,3-dihydroxynaphthalene-functionalized Amberlite XAD-4 resin: Applications for the separation and preconcentration of trace metal ions prior to their determination by inductively coupled plasma atomic emission spectrometry

A simple, sensitive column solid-phase extraction procedure for separation and preconcentration of Cu(II), Ni(II), Co(II), and Cd(II) in spiked and natural water samples using 2,3-dihydroxynaphthalene-functionalized Amberlite XAD-4 (XAD-4-DHN) chelating resin prior to their determination by inductively coupled plasma atomic emission spectrometry was discussed. The optimum experimental parameters such as pH, volume of sample and eluent, flow-rates of uptake and stripping, and sorption capacity of the chelating resin, were evaluated. The effect of the electrolytes and the cations on the preconcentration of metal ions was also investigated. The chelating resin could be reused for more than 20 cycles of sorption–desorption without any significant change (<1.0%). Recoveries obtained from this method range from 96 to 102% with R.S.D of 2.50 (n = 4). The detection limits for Cu(II), Ni(II), Co(II), and Cd(II) were found to be 1.9, 0.9, 1.2 µg, and 1.4 µg L−1, respectively. The proposed method was applied for the determination of Cu(II), Ni(II), Co(II), and Cd(II) in spiked, tap water, and river water samples.

Determination of bismuth in natural water samples by ICP-AES after preconcentration on dithiocarbamates-coated amberlite XAD-7

A column solid-phase extraction procedure for separation and preconcentration of bismuth in natural water samples using sodium diethyldithiocarbamate (NaDTTC) or piperidene dithiocarbamate (pipDTC)-coated Amberlite XAD-7 resin prior to their determination by inductively coupled plasma atomic emission spectrometry (ICP-AES) is reported. The results showed that solution pH and flow rate would affect the sorption of bismuth. The sorbed bismuth was eluted with 4 M/L of HNO3. The extractor system has good sorption capacity values of 9.82 mg/g of Bi on NaDTTC-coated resin and 9.56 mg/g of Bi on pipDTC-coated resin. The preconcentration factor was 150 and 170 for pipDTC-coated resin and NaDTTC-coated resin, respectively. The detection limits are 0.9 and 1.2 µg/L for resin-coated with NaDTTC and pipDTC, respectively. The results showed that resin coated with NaDTTC performs slightly better in the recovery of bismuth than resin coated with pipDTC. The accuracy of the proposed method was investigated by determining the bismuth in spiked water samples. The relative standard deviations of the determination of bismuth were below 5%. The proposed procedure was applied for the determination of bismuth in natural water and seawater samples.

Estimating non‐crystalline and crystalline aluminum and iron by selective dissolution in a riparian forest soil

Abstract We compared sequential and separate extraction procedures for estimating non‐crystalline and crystalline aluminum (Al) and iron (Fe) in a floodplain forest soil. We used 0.2M acid ammonium oxalate (pH 3.0) to estimate non‐crystalline Al and Fe, dithionite‐citrate‐bicarbonate to estimate crystalline Fe, and 0.1M sodium hydroxide (NaOH) to estimate crystalline Al. Both separate and various combinations of sequential extractions were compared, as well as variations in soil:solution ratio, extraction time, extraction temperature, and the use of field‐moist versus dried soils. A sequential oxalate/NaOH extraction, using 0.4 g dry weight equivalent of field‐moist soil and a soil:solution ratio of 1:100, gave the best estimate of non‐crystalline Al and Fe and crystalline Al, while a separate 16 hour DCB extraction at room temperature, using 0.8 g dry weight equivalent of field‐moist soil and a soil:solution ratio of 1:50, gave the best estimate for non‐crystalline plus crystalline Fe. A sequential oxala...

Effective high-performance liquid chromatographic determination of glafenine in plasma: Pharmacokinetic application

A high-performance liquid chromatograpic method for an effective determination ofglafenine and its main metabolite, glafenic acid, is described. The assay involves separate extraction procedures for glafenine and for its metabolite, but the same internal standard (floctafenine) and the same chromatographic conditions (including a 5-μm C 8 column, a quaternary solvent mixture of water—acetonitrile—diethylamine—acetic acid and an ultraviolet detector set at 360 nm). For 1 ml of plasma, the detection limit is 0.05 mg/l for glafenine and 0.25 mg/l for glafenic acid. Compared with previously described techniques, this assay uses a very low glafenine linearity range, which allows the true pharmacokinetics of this drug to be described for the first time.

Reversed-Phase High Performance Liquid Chromatographic Determination of Carbaryl in Postmortem Specimens

A reversed-phase high performance liquid chromatographic (HPLC) method has been developed for the analysis of carbaryl in postmortem samples. It involves the use of an aqueous acetonitrile mobile phase to give rapid, reproducible analyses and an external standard for quantitation. Two separate extraction procedures (Extrelut column and protein precipitation with acetonitrile) are described; each one is suited to a particular substrate and each one leads to an almost complete recovery of carbaryl from that substrate.

Stabilized Normal-Phase High-Performance Liquid Chromatographic Analysis of Aspirin and Salicylic Acid in Solid Pharmaceutical Dosage Forms

A simultaneous analysis of aspirin and nonaspirin salicylates in solid pharmaceutical dosage forms is described. Two separate extraction procedures are employed, one for plain aspirin tablets and one for tablets containing aspirin plus buffers or antacids. The analyses of the extracted samples are accomplished by a stabilized normal-phase high-performance liquid chromatographic (HPLC) procedure. Prepared samples and standards are stable for up to 24 h, and the methodology is suitable for an automated HPLC system.

Qualitative Analysis of Propyl Gallate, Nordihydroguaiaretic Acid, Butylated Hydroxyanisole, and Butylated Hydroxytoluene in Fats and Oils

Abstract collaborative study was made of qualitative tests for added antioxidants in oils and fats. Samples of corn oil, edible tallow, and lard to which 5, 5, 10, and 15 ppm of propyl gallate, butylated hydroxyanisole, butylated hydroxytoluene, and nordihydroguaiaretic acid, respectively, had been added, plus blank samples of the oil and the fats were analyzed by 9 collaborators. The tests employed were previously described in This Journal, 45, 244 (1962). The present report includes an extraction procedure for separation of individual antioxidants, after which the qualitative tests are applied. All collaborators identified the added antioxidants correctly. (Four of the nine repeated the analyses of the samples, which were resubmitted to them in different sequence and with different identifications.) The procedure is considered suitable for routine screening, since oils and fats in commercial use contain a considerably higher level of antioxidants than were added to these collaborative samples.