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Phase Extraction (phase + extraction)
Kinds of Phase Extraction Selected AbstractsRemoval and Recovery of UO2(??) from Water Samples Using 2,2,-Diamino-4,4,-bithiazole as a New Reagent for Solid Phase ExtractionCHINESE JOURNAL OF CHEMISTRY, Issue 4 2010Majid Soleimani Abstract A novel sensitive and simple method for rapid and selective extraction, preconcentration and determination of uranyl as its 2,2,-diamino-4,4,-bithiazole (DABTZ) complex by using octadecylsilica columns and spectrophotometry is presented. Extraction efficiency and the influence of flow rates of sample solution and eluent, pH, amount of DABTZ, type and least amount of eluent for elution of uranyl complex from columns, break-through volume and limit of detection were evaluated. Also the effects of various cationic and anionic interferences on percent recovery of uranyl were studied. Average extraction efficiency of ca. 90% was obtained by elution of the column with minimal amount of solvent in the presence of interferences. The average preconcentration factor, 136 and a detection limit 0.32 ng·mL,1 were obtained. The method was applied to the recovery and determination of uranyl in different water samples. [source] Solid Phase Extraction of Thallium(III) on Micro Crystalline Naphthalene Modified with N,N, -Bis(3-methylsalicylidene)- ortho -phenylenediamine and Determination by SpectrophotometryCHINESE JOURNAL OF CHEMISTRY, Issue 10 2008Ali MOGHIMI Abstract A novel, simple, sensitive and effective method has been developed for preconcentration of thallium on N,N, -bis(3-methylsalicylidene)- ortho -phenylenediamine (MSOPD) adsorbent in a pH range 5.0,10.0, prior to its spectrophotometric determination, based on the oxidation of bromopyrogallol red at ,=520 nm. This method makes it possible to quantitize thallium in a range of 3.6×10,9 to 2.0×10,5 mol/L, with a detection limit (S/N=3) of 1.42×10,9 mol/L. This procedure has been successfully applied to determine the ultra trace levels of thallium in the environmental samples, free from the interference of some diverse ions. The precision, expressed as relative standard deviation of three measurements, is better than 2.9%. [source] Methods for detecting and identifying retinoids in tissueDEVELOPMENTAL NEUROBIOLOGY, Issue 7 2006Thomas E. Gundersen Abstract Methods for retinoid analysis in tissue include direct spectrophotometry or fluorometry and retinoid responsive reporter constructs in the form of cell reporter assays or transgenic reporter animals, but chromatographic methods dominate and posses several superior features in quantitative analysis. The multitude of extraction protocols used can coarsely be divided into manual liquid-liquid extraction protocols and semi- or fully automated solid phase extraction-based protocols. Liquid chromatographic separation in reversed phase dominates although normal phase is also used. Detection is mainly performed with UV detectors although electrochemical and fluorescence detection is also used. Mass spectrometry in combination with LC is more often used in retinoid analysis and is likely to dominate in the future. © 2006 Wiley Periodicals, Inc. J Neurobiol 66: 631,644, 2006 [source] Bioreactor for cultivation of red beet hairy roots and in situ recovery of primary and secondary metabolitesENGINEERING IN LIFE SCIENCES (ELECTRONIC), Issue 3 2009Bhagyalakshmi Neelwarne Abstract To arrive at an appropriate bioreactor design and in situ recovery of the products, red beet hairy roots were used as a model system where the levels of betalain pigments (betacyanins and betaxanthins) were followed as secondary metabolite and the peroxidase enzyme as primary metabolite. Medium volume and other kinetic parameters were found to play significant roles by way of directly affecting the biomass yield rather than a specific metabolite. The hydrodynamic stress created on the roots by large culture volume could be minimized by pulse-feeding of medium in shake-flasks; and by separating the biomass chamber from the aerated medium reservoir in circulatory fed-batch bioreactor. Accordingly the bioreactor was modified to provide anchorage and air-enrichment chamber which resulted in higher formation of both the metabolites than in shake-flasks. Various down-stream processing aspects such as in situ release of pigments by non-destructive methods, followed by adsorption through a column and recovery by desorption were optimized for betalains. A strategy for simultaneous recovery of pigment and peroxidase was worked out using aqueous two phase extraction (ATPE). [source] Assessing exposure of sediment biota to organic contaminants by thin-film solid phase extractionENVIRONMENTAL TOXICOLOGY & CHEMISTRY, Issue 2 2009Lizanne M. Meloche Abstract Differences in bioavailability among sediments are a source of variability and uncertainty in sediment quality assessment. We present three sets of studies designed to test a thin-film solid phase extraction technique for characterizing the bioavailability of organic chemicals in sediments. Laboratory studies with spiked natural sediments reveal highly reproducible thin-film extractions for chemicals with octanol,water partition coefficients between 104.5 and 108.5, with 95% equilibration times between 1 and 600 h. Studies with field-collected sediments illustrate that method detection limits are sufficiently low for field application at contaminated sites. Bioaccumulation studies with clams (Macoma balthica) show excellent correlations between thin-film and animal tissue concentrations. We conclude that thin-film extraction provides an ecologically relevant, fugacity-based measure of chemical exposure that can be expected to improve sediment quality assessments. [source] Wastewater treatment polymers identified as the toxic component of a diamond mine effluentENVIRONMENTAL TOXICOLOGY & CHEMISTRY, Issue 9 2004Simone J. C. de Rosemond Abstract The EkatiÔ Diamond Mine, located approximately 300 km northeast of Yellowknife in Canada's Northwest Territories, uses mechanical crushing and washing processes to extract diamonds from kimberlite ore. The processing plant's effluent contains kimberlite ore particles (,0.5 mm), wastewater, and two wastewater treatment polymers, a cationic polydiallydimethylammonium chloride (DADMAC) polymer and an anionic sodium acrylate polyacrylamide (PAM) polymer. A series of acute (48-h) and chronic (7-d) toxicity tests determined the processed kimberlite effluent (PKE) was chronically, but not acutely, toxic to Ceriodaphnia dubia. Reproduction of C. dubia was inhibited significantly at concentrations as low as 12.5% PKE. Toxicity identification evaluations (TIE) were initiated to identify the toxic component of PKE. Ethylenediaminetetraacetic acid (EDTA), sodium thiosulfate, aeration, and solid phase extraction with C-18 manipulations failed to reduce PKE toxicity. Toxicity was reduced significantly by pH adjustments to pH 3 or 11 followed by filtration. Toxicity testing with C. dubia determined that the cationic DADMAC polymer had a 48-h median lethal concentration (LC50) of 0.32 mg/L and 7-d median effective concentration (EC50) of 0.014 mg/L. The anionic PAM polymer had a 48-h LC50 of 218 mg/L. A weight-of-evidence approach, using the data obtained from the TIE, the polymer toxicity experiments, the estimated concentration of the cationic polymer in the kimberlite effluent, and the behavior of kimberlite minerals in pH-adjusted solutions provided sufficient evidence to identify the cationic DADMAC polymer as the toxic component of the diamond mine PKE. [source] Determination of cypermethrin in palm oil matricesEUROPEAN JOURNAL OF LIPID SCIENCE AND TECHNOLOGY, Issue 10 2009Badrul Hisyam Zainudin Abstract In this study, a new method was developed for the determination of cypermethrin residue in both crude palm oil (CPO) and crude palm kernel oil (CPKO) using GC with electron capture detector. In this method, the oil was extracted with acetonitrile. Aliquots were cleaned-up using combined solid phase extraction (SPE), and a primary-secondary amine in combination with graphitized carbon black. The SPE cartridges were first conditioned and then eluted with acetonitrile. Cypermethrin recoveries from the fortified CPO samples were 87,98% with relative standard deviation (RSD) values of 4,8%, while those for the fortified CPKO samples were 83,100% with RSD values of 3,10%. Since good recoveries were obtained with RSD values below 10% in most cases, the proposed methodology will be useful for the analyses of palm oil samples. The method was successfully applied to the analysis of cypermethrin in real palm oil samples from various parts of Malaysia. No cypermethrin residue was found among 30 samples analyzed. [source] PHENOLIC COMPOUNDS, TOCOPHEROLS AND OTHER MINOR COMPONENTS IN VIRGIN OLIVE OILS OF SOME TUNISIAN VARIETIESJOURNAL OF FOOD BIOCHEMISTRY, Issue 2 2007D. KRICHENE ABSTRACT The phenols, ,-tocopherols, fatty acids and oxidative stability of six monovarietal virgin olive oils (VOOs) were determined. Fourteen phenolic compounds were detected and quantified by solid phase extraction and reversed phase-high performance liquid chromatography. Dialdehydic form of elenolic acid linked to tyrosol and hydroxytyrosol, oleuropein and ligstroside aglycones were the main components in all samples. Pinoresinol was the most abundant component in lignan fraction. The total phenol content of these monovarietal oils varied from 66.82 mg/kg in "Neb Jmel" oil to 662.74 mg/kg in "El Hor" oil. A wide range of ,-tocopherol contents was also noticed; it varied from 141.94 mg/kg in "Semni" variety to 364.23 mg/kg in "Jdallou" variety. With regard to pigments, chlorophylls and carotenoids were found at variable concentrations: with median values of 11.33 and 3.10 mg/kg, respectively. Among the studied varieties, "Oueslati" and El Hor were characterized by the lowest levels of palmitic and linoleic acids and the highest values of oleic acid. [source] EFFECTS OF COOKED TEMPERATURES AND ADDITION OF ANTIOXIDANTS ON FORMATION OF HETEROCYCLIC AROMATIC AMINES IN PORK FLOSSJOURNAL OF FOOD PROCESSING AND PRESERVATION, Issue 2 2009GUOZHOU LIAO ABSTRACT Heterocyclic aromatic amines (HAAs) are an important class of food mutagens and carcinogens produced in meats cooked at high temperature. The formation of HAAs in pork floss during processing and the effect of vitamin C and vitamin E on HAAs formation in pork floss were studied. Pork floss was prepared by steaming of raw pork, followed by pressing, tearing, adding various additives, and then the cooked pork was subjected to stir frying. The various HAAs in pork floss were isolated by solid phase extraction and analyzed by high-performance liquid chromatography (HPLC). Results showed that the type and level of HAAs increased with increasing processing temperature. Up to seven HAAs, 9H-pyrido[4,3-b]indole (Norharman), 1-methyl-9H-pyrido[4,3-b]indole (Harman), 2-amino-1- methyl-6-phenylimidazo[4,5-f]pyridine (PhIP), 2-amino-dipyrido[1,2-a: 3,,2,-d]imidazole (Glu-P-2), 3-amino-1-methyl-5H-pyrido[4,3-b]indole (Trp-P-2), 2-amino-9H-pyrido[2,3-b]indole (AaC) and 2-amino-3-methyl-9H-pyrido[2,3-b]indole (MeAaC) were detected in pork floss when stir fried at 150C. Color development increased with cooking temperatures, and was correlated with HAAs formation. The addition of vitamin C at various levels was not effective toward HAAs inhibition. However, the incorporation of 0.1% vitamin E reduced Norharman, PhIP, AaC and MeAaC concentrations in the pork floss. PRACTICAL APPLICATION The formation of heterocyclic aromatic amines (HAAs) is one of the most unfavorable changes during the cooking of food. Since the connection between the consumption of dietary carcinogens and cancer risks in human has been established, interest in this matter has been growing. However, the processing methods and conditions of Chinese traditional food are different from Western, and to date, little is known about HAAs content in the traditional meat products of China. The information derived from this study serves as an essential base of knowledge from a public health standpoint, and contributes to a repository of HAAs information relevant to Chinese cooking; it also can provide clues to understanding the factors that affect HAAs formation and can indicate means of reducing or eliminating these compounds. [source] Lipase-mediated Acidolysis of Fully Hydrogenated Soybean Oil with Conjugated Linoleic AcidJOURNAL OF FOOD SCIENCE, Issue 1 2004J. Ortega ABSTRACT: Interesterification (acidolysis) of fully hydrogenated soybean oil (melting point = 69.9 °C) with conjugated linoleic acid (CLA) was carried out in a batch reactor at 75 °C. Lipases from Candida antarctica, Rhizomucor miehei, Pseudomonas sp., and Thermomyces lanuginosus were used at 5% (wt/wt) of the total substrate load. The lipase from Rhizomucor miehei produced the fastest reaction rates, and the greatest extent of incorporation of CLA residues in acylglycerols was achieved in 12 h. Lipases from C. antarctica and T. lanuginosus produced slower initial rates, and maximum extents of incorporation of CLA residues were achieved in 24 h. The lipase from Pseudomonas sp. produced the slowest initial rate. The corresponding maximum extent of incorporation was reached in 48 h. Differential scanning calorimetry analysis of the triacylglycerol (TAG) fractions produced by C. antarctica, R. miehei, and T. lanuginosus lipases after purification by solid phase extraction showed little variation in melting point (60.4 °C, 62.8 °C, and 60.1 °C, respectively). By contrast, the corresponding TAG fraction produced by the Pseudomonas sp. lipase melted at 48.4 °C. The positional distribution of the TAGs produced by the lipase from Pseudomonas sp. differed appreciably from those produced by the other enzymes. [source] Representativeness of Apple Aroma Extract Obtained by Vacuum Hydrodistillation: Comparison of Two Concentration TechniquesJOURNAL OF FOOD SCIENCE, Issue 8 2003E. Mehinagic ABSTRACT: Vacuum hydrodistillation, which is a very gentle work-up procedure, has never been used for the extraction of apple aroma. During the concentration of aroma that follows vacuum hydrodistillation, some very volatile components can be lost. The aim of this study was to compare 2 different concentration techniques, liquid-liquid extraction and solid phase extraction, to obtain an apple aroma extract as close as possible to fresh apple. After the elimination of solvent from the extract by gas chromatography, the study of the odor characteristics of solvent-free extracts was made possible. Vacuum hydrodistillation was convenient for fresh apples. [source] Development of a Quantitative LC-MS/MS Method for the Analysis of Common Propellant Powder Stabilizers in Gunshot Residue,JOURNAL OF FORENSIC SCIENCES, Issue 4 2007Désiré Laza Ph.D. Abstract:, In traditional scanning electron microscopy/energy dispersive X-ray analysis of gunshot residue (GSR), one has to cope more and more frequently with limitations of this technique due to the use of lead-free ammunition or ammunition lacking heavy metals. New methods for the analysis of the organic components of common propellant powder stabilizers were developed based on liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). A multiple reactions monitoring scanning method was created for the screening of akardite II, ethylcentralite, diphenylamine, methylcentralite, N-nitrosodiphenylamine, 2-nitrodiphenylamine, and 4-nitrodiphenylamine, present in standards mixtures. Five out of seven of these target compounds can be selectively identified and distinguished from the two others with a high accuracy. Samples from the hands of a shooter were collected by swabbing and underwent solid phase extraction prior to analysis. Detection limits ranging from 5 to 115 ,g injected were achieved. Results from several firing trials show that the LC-MS/MS method is suitable for the detection of stabilizers in samples collected following the firing of 9 mm Para ammunitions. [source] Two-step radiosynthesis of [18F]N -succinimidyl-4-fluorobenzoate ([18F]SFB)JOURNAL OF LABELLED COMPOUNDS AND RADIOPHARMACEUTICALS, Issue 8 2009Matthias Glaser Abstract The acylation reagent [18F]N -succinimidyl-4-fluorobenzoate (18F-SFB) has been prepared using a new two-step approach. The starting material p- [18F]fluorobenzaldehyde (18F-FBA) was obtained by an improved radiosynthesis with a decay-corrected radiochemical yield of 66±6 % (n=3). Reaction of 18F-FBA with (diacetoxyiodine)benzene and N -hydroxysuccinimide and preparative HPLC purification furnished 18F-SFB in an r.c.y. of 49±6 % (n=3), based on the starting radioactivity of 18F-FBA. The radiochemical purity of 18F-SFB was >99%. Alternatively, purification by solid phase extraction gave 18F-SFB with an r.c.y. of 77±9% (n=4) and a radiochemical purity of 89±5% (n=4). This radiochemical synthesis only used non-aqueous solvents, which simplifies the method and facilitates subsequent applications of 18F-SFB. Copyright © 2009 John Wiley & Sons, Ltd. [source] Radiosynthesis of novel 18F-labelled derivatives of indiplon as potential GABAA receptor imaging tracers for PETJOURNAL OF LABELLED COMPOUNDS AND RADIOPHARMACEUTICALS, Issue 3 2008Steffen Fischer Abstract The involvement of gamma amino butyric acid (GABA) receptors in a variety of neurological and psychiatric diseases has promoted the development and use of radiolabelled benzodiazepines (BZ) for brain imaging by PET. However, these radioligands are unable to distinguish between the various subtypes of GABAA receptors. Novel non-BZ such as the pyrazolo-pyrimidine indiplon proved to be selective for the ,1 -subunit of the GABAA receptor. Here, we describe the syntheses of four novel 18F-labelled indiplon derivatives. Radiosyntheses were performed via n.c.a. 18F-nucleophilic substitution starting from the tosyl, bromo, and 4-nitrobenzoyl precursors to obtain fluorine substituted N -alkylamide side chain derivatives of indiplon, followed by multistep purification using semi-preparative high-performance liquid chromatography and solid phase extraction. Tosyl and bromo precursors were converted into 18F-labelled indiplon derivatives with good and reproducible radiochemical yield (RCY) (35,70%, decay corrected), high radiochemical purity (,98.5%), and high specific activity (,>,150,GBq/µmol). By contrast, a low RCY (5,10%) and specific activity (10,15,GBq/µmol) were achieved for the 4-nitrobenzoyl precursor. Copyright © 2008 John Wiley & Sons, Ltd. [source] Synthesis of a technetium-99m labelled L -tyrosine derivative with the fac - 99mTc(I)(CO)3 -core using a simple kit-procedureJOURNAL OF LABELLED COMPOUNDS AND RADIOPHARMACEUTICALS, Issue 8 2004Ralf Schirrmacher Abstract The synthesis of a novel technetium-99m labelled derivative of L -tyrosine as a potential tumour imaging agent for nuclear medicine diagnosis is reported. The synthesis involved the labelling precursor fac -[99mTc(OH2)(CO)3]+ which was synthesized using the commercially available Isolink® -labelling kit and the tyrosine derivative O-(N,N-bis(carboxymethyl)aminoethyl)- L -tyrosine trifluoroacetate. The labelled compound O -(99mTc(I)-tricarbonyl- N,N-bis(carboxymethyl)aminoethyl)- L -tyrosine was obtained in a radiochemical yield of 70,80% within 60 min with a radiochemical purity greater than 98% without any HPLC purification step. Purification was achieved merely by solid phase extraction. Chemical as well as chiral purity was determined using gradient- and chiral HPLC. Copyright © 2004 John Wiley & Sons, Ltd. [source] Synthesis and evaluation of tritium labelled 10-methylgalanthamine iodide: a novel compound to examine the mechanism of interaction of galanthamine derivatives with the nicotinic acetylcholine receptorsJOURNAL OF LABELLED COMPOUNDS AND RADIOPHARMACEUTICALS, Issue 12 2003Andreas Schildan Abstract A new promising galanthamine derivative, 10-[3H]methylgalanthamine iodide, was synthesized for binding studies to nicotinic acetylcholine receptors expressed in Torpedo electric ray electroplaques. Galanthamine was reacted with [3H]methyl iodide to yield 10-[3H]methylgalanthamine iodide with a radiochemical yield of >70% and a specific activity of 32 Ci/mmol after purification via solid phase extraction. To test the ligand properties of the radioligand, calcium imaging and electrophysiology of the non-radioactive analogue were performed to obtain an EC50 of 270 nM, a Hill coefficient of 1.9 and the induced cell current. Copyright © 2003 John Wiley & Sons, Ltd. [source] A combined loop-SPE method for the automated preparation of [11C]doxepinJOURNAL OF LABELLED COMPOUNDS AND RADIOPHARMACEUTICALS, Issue 4 2002R. Iwata Abstract A simple and versatile loop-solid phase extraction (SPE) method was developed for the automated preparation of [11C]doxepin, a histamine H1 receptor antagonist, from [11C]methyl triflate ([11C]MeOTf). This labeling agent was passed through a Teflon or Tefzel loop coated internally with a film of the precursor solution. The reaction products were then flushed from the loop to a short SPE column, where they were concentrated and then injected onto a semi-preparative HPLC column simply by switching an injection valve. By applying this combined loop-SPE technique the whole procedure turned out to be easily automated. The formation of [11C]methylated doxepin ([11C]methyldoxepin) was observed and the ratio of doxepin to methyldoxepin was found to be clearly correlated with the mass ratio of nordoxepin to MeOTf. This observation highlights the importance of [11C]MeOTf specific activity in the [11C]methylation of secondary amines. Using this method, [11C]Doxepin was prepared in over 40% radiochemical yield from high specific activity [11C]MeOTf. Copyright © 2002 John Wiley & Sons, Ltd. [source] LC,ESI-MS/MS analysis for the quantification of morphine, codeine, morphine-3-,- D -glucuronide, morphine-6-,- D -glucuronide, and codeine-6-,- D -glucuronide in human urineJOURNAL OF MASS SPECTROMETRY (INCORP BIOLOGICAL MASS SPECTROMETRY), Issue 11 2005Constance M. Murphy Abstract A liquid chromatographic-electrospray ionization-tandem mass spectrometric method for the quantification of the opiates morphine, codeine, and their metabolites morphine-3-,- D -glucuronide (M-3-G), morphine-6-,- D -glucuronide (M-6-G) and codeine-6-,- D -glucuronide (C-6-G) in human urine has been developed and validated. Identification and quantification were based on the following transitions: 286 to 201 and 229 for morphine, 300 to 215 and 243 for codeine, 644 to 468 for M-3-G, 462 to 286 for M-6-G, and 476 to 300 for C-6-G. Calibration by linear regression analysis utilized deuterated internal standards and a weighting factor of 1/X. The method was accurate and precise across a linear dynamic range of 25.0 to 4000.0 ng/ml. Pretreatment of urine specimens using solid phase extraction was sufficient to limit matrix suppression to less than 40% for all five analytes. The method proved to be suitable for the quantification of morphine, codeine, and their metabolites in urine specimens collected from opioid-dependent participants enrolled in a methadone maintenance program. Copyright © 2005 John Wiley & Sons, Ltd. [source] Impurities in a morphine sulfate drug product identified as 5-(hydroxymethyl)-2-furfural, 10-hydroxymorphine and 10-oxomorphineJOURNAL OF PHARMACEUTICAL SCIENCES, Issue 3 2003Seán S. Kelly Abstract Stability testing of morphine sulfate formulated with nonpareil sugar seeds (consisting of sucrose and starch) and fumaric acid revealed the formation of the three impurities 5-(hydroxymethyl)-2-furfural, 10-hydroxymorphine and 10-oxomorphine. 5-(Hydroxymethyl)-2-furfural was isolated via semipreparative HPLC utilizing volatile mobile phase constituents and was identified by analysis of its HRMS and NMR spectra. 10-Hydroxymorphine and 10-oxomorphine were obtained via semipreparative HPLC and subsequent removal of ion-pair reagents using an anion exchange resin, or by solid phase extraction, and identified by spectroscopic analysis followed by comparison with authentic materials. 5-(Hydroxymethyl)-2-furfural is a degradation product of hexose sugars, and its formation in the presence of morphine sulfate formulated with fumaric acid suggests that caution should be exercised when including nonpareil seeds in formulations that contain acidic drug salts and/or acid excipients. The preliminary results of tests on the interaction of acidic salts of some other drugs with nonpareil seeds are presented. © 2003 Wiley-Liss, Inc. and the American Pharmaceutical Association J Pharm Sci 92:485,493, 2003 [source] Purification and identification of an impurity in bulk hydrochlorothiazideJOURNAL OF PHARMACEUTICAL SCIENCES, Issue 11 2001Xueguang Fang Abstract Hydrochlorothiazide (6-chloro-3,4-dihydro-2H-1,2,4-benzothiadiazine-7-sulfonamide 1,1-dioxide) (HCTZ) 1 is a widely used diuretic and anti-hypertensive. Recently, the Pharmeuropa recognized a new impurity initially thought to be an HCTZ dimer 6, which consists of the active drug (HCTZ) linked via the former ,-ring methylene to a known degradate, 5-chloro-2,4-disulfamylaniline 2. In an effort to meet a new requirement, an analytical high-pressure liquid chromatography method was developed that was selective and sensitive to the subject impurity. The impurity was concentrated and purified using a combination of solid phase extraction and reverse-phase high-pressure liquid chromatography. Subsequently, the impurity has been identified as a specific HCTZ-CH2 -HCTZ isomer utilizing a variety of analytical techniques, including hydrolysis, ultraviolet spectroscopy, liquid chromatography/mass spectrometry, and 1H and 13C nuclear magnetic resonance (NMR) spectroscopy. The data resulting from the application of these analytical techniques confirm the identity of the impurity as a methylene bridged pair of HCTZ molecules; however, a total of six possible isomers 7a,f exist because of the presence of three reactive amines/sulfonamides on each HCTZ molecule. One unique molecular structure (4-[{6-chloro-3,4,-dihydro-2H-1,2,4-benzothiadiazine-7-sulfonamide-1,1-dioxide}-methyl]-chloro-3-hydro-H-1,2,4-benzothiadiazine-7-sulfonamide-1,1-dioxide) 7f was identified using two-dimensional COSY, NOESY, and TOCSY 1H NMR experiments. © 2001 Wiley-Liss, Inc. and the American Pharmaceutical Association J Pharm Sci 90:1800,1809, 2001 [source] Determination of methylene blue residues in aquatic products by liquid chromatography-tandem mass spectrometryJOURNAL OF SEPARATION SCIENCE, JSS, Issue 23-24 2009Jin-Zhong Xu Abstract A method for the determination and confirmation of methylene blue (MB) in aquatic products was developed. Residues of MB were extracted from homogenized tissues with acetonitrile/sodium acetate buffer solution, and simply cleaned up with dichloromethane liquid/liquid extraction. After concentration and dissolution, the sample solutions were cleaned up by the neutral alumina and weak cation-exchange solid phase extraction (SPE) cartridge, prior to LC-MS/MS analysis. MB was determined at 1.0,20,,g/kg in eel, toasted eel and shrimp, with a limit of quantification of 0.5,,g/kg. Recovery for MB was between 73.0% and 108.3%. This method is fast, exact and sensitive. It can be applied to determine MB in aquatic products. [source] Multiresidue HPLC analysis of ten quinolones in milk after solid phase extraction: Validation according to the European Union Decision 2002/657/ECJOURNAL OF SEPARATION SCIENCE, JSS, Issue 15 2007Eleni A. Christodoulou Abstract A rapid and sensitive analytical method was developed for the residue analysis of ten quinolones (enoxacin (ENO), ofloxacin (OFL), norfloxacin (NOR), ciprofloxacin (CIP), danofloxacin (DAN), enrofloxacin (ENR), sarafloxacin (SAR), oxolinic acid (OXO), nalidixic acid (NAL), and flumequine (FLU)) in cow's milk. The analytes were extracted from milk by a deproteinization step followed by a simple SPE cleanup procedure using LiChrolut RP-18 Merck cartridges. Recoveries varied between 75 and 92%. HPLC separation was performed at 25°C using an ODS-3 PerfectSil® Target (250×4 mm2) 5 ,m analytical column (MZ-Analysentechnik, Germany). The mobile phase consisted of a mixture of TFA 0.1%,CH3CN,CH3OH, delivered by a gradient program at the flow rate of 1.2 mL/min. Elution of the ten analytes and the internal standard (caffeine, 7.5 ng/,L) was completed within 27 min. Column effluent was monitored using a photodiode array detector, set at 275 and 255 nm. The developed method was validated according to the criteria of Commission Decision 2002/657/EC. The LODs of the specific method of quinolones' determination in milk varied between 1.5 and 6.8 ng/,L. [source] Potential sources of background contaminants in solid phase extraction and microextractionJOURNAL OF SEPARATION SCIENCE, JSS, Issue 7 2007Robert Stiles Abstract A study to identify the sources of background contamination from SPE, using a C-18 sorbent, and solid-phase microextraction (SPME), using a 70 ,m carbowax/divinylbenzene (CW/DVB) fiber, was carried out. To determine the source of contamination, each material used in the procedure was isolated and examined for their contribution. The solid-phase column components examined were: sorbent material and frits, column housings and each solvent used to elute analytes off the column. The components examined in the SPME procedure were: SPME fiber, SPME vials, water (HPLC grade), and salt (sodium chloride) used to increase the ionic strength. The majority of the background contaminants from SPE were found to be from the SPE sorbent material and frits. The class of contaminants extracted during a blank extraction were phthalates and other plasticizers used during the manufacturing process. All had blank levels corresponding to measured concentrations below 2 ng/mL, except for undecane, which had a concentration of 5.4 ng/mL. The most prevalent contaminants in the SPME blank procedure are 1,9-nonanediol, a mixture of phthalates and highly bis- substituted phenols. All the concentrations were below 2 ng/mL, with the exception of bis (2-ethylhexyl) phthalate, which had concentrations ranging from 5 to 20 ng/mL. [source] Comparison of various extraction techniques for isolation and determination of isoflavonoids in plantsJOURNAL OF SEPARATION SCIENCE, JSS, Issue 1 2007Bajer Abstract In the present paper, the following extraction techniques have been used for extracting isoflavonoids from the species Matricaria recutita, Rosmarinus officinalis, Foeniculum vulgare, and Agrimonia eupatoria L.: supercritical fluid extraction (SFE), pressurized fluid extraction, matrix solid phase dispersion, ultrasonic extraction in an ultrasonic bath (USE) and by means of an ultrasonic homogeniser (HOM), extraction by means of Soxhlet apparatus (SOX), and solid phase extraction. Experimental optimization of all techniques has been carried out using a soybean flour. Subsequent analyses of the extracts were carried out by liquid chromatography with UV detection. The maximum yields of daidzein and genistein were obtained by extraction with the SOX, USE, and HOM techniques. The maximum yields of apigenin and biochanin A from herb samples were obtained by SFE. [source] Ultratraces analysis of organochlorine pesticides in drinking water by solid phase extraction coupled with large volume injection/gas chromatography/mass spectrometryJOURNAL OF SEPARATION SCIENCE, JSS, Issue 17 2005Silvia H. G. Brondi Abstract This study describes an SPE coupled with large volume injection (LVI) analytical method for the analysis of organochlorine pesticides, BHC (,, ,, ,), aldrin, endosulfan (,, ,), endrin, dieldrin, and DDT, from aqueous samples. Determination was carried out by GC with MS. The LODs of organochlorine pesticides were determined at 10 ng/L concentration levels, and the results show that SPE-LVI-GC/MS has the potential to accurately determine organochlorine pesticides in water, as it avoids analyte classes in the various steps of a typical extraction procedure. [source] Determination of cholesterol oxides content in milk products by solid phase extraction and gas chromatography-mass spectrometryJOURNAL OF SEPARATION SCIENCE, JSS, Issue 9-10 2003María V. Calvo Abstract A method for quick and reliable analysis of cholesterol oxidation products (COPs) in dairy products has been developed. After lipid extraction, fat was transesterified under mild conditions to avoid degradation of the target compounds. Isolation of the COPs studied from other components in the lipid fraction was carried out on an aminopropyl SPE cartridge. Finally, analytes were analysed by GC-MS without derivatisation. The method developed provides high specificity and good sensitivity, allowing the direct and unambiguous determination of the underivatized COPs investigated. Application of the method to dairy food analysis revealed the presence of COPs in powder milks and milk-based infant formulas commercially available in Spain, showing that attention should be focused on reduction of cholesterol oxidation levels during both the processing and the storage of these types of foodstuffs. [source] Selective determination of famotidine in human plasma by high performance liquid chromatography in alkaline media with solid phase extractionJOURNAL OF SEPARATION SCIENCE, JSS, Issue 8 2003Eva Anzenbacherová Abstract A new method is described for the determination of famotidine by solid phase extraction from alkalinized human plasma followed by reversed phase (RP) HPLC in acetonitrile/alkaline buffer with molsidomine as an internal standard. Different acetonitrile/aqueous buffer mobile phases as well as various RP columns were used. Alkaline medium allowed the limit of quantitation to be lowered to 5 ng/mL of plasma as the famotidine gives more intense absorption at about 286 nm (at pH values higher than 7). Moreover, work in alkaline media and at this wavelength is highly selective as peaks corresponding to impurities present in most samples are well separated. A method using a mildly alkaline mobile phase (acetonitrile/10 mM phosphate with 10 mM 1-heptanesulphonic acid, pH 7.5) was successfully used for determination of famotidine in human plasma in a pharmacokinetic study. [source] Moxidectin and ivermectin metabolic stability in sheep ruminal and abomasal contentsJOURNAL OF VETERINARY PHARMACOLOGY & THERAPEUTICS, Issue 5 2005A. LIFSCHITZ The oral administration of macrocyclic lactones to sheep leads to poorer efficacy and shorter persistence of the antiparasitic activity compared to the subcutaneous treatment. Gastrointestinal biotransformation occurring after oral treatment to ruminant species has been considered as a possible cause of the differences observed between routes of administration. The current work was addressed to evaluate on a comparative basis the in vitro metabolism of moxidectin (MXD) and ivermectin (IVM) in sheep ruminal and abomasal contents. Both compounds were incubated under anaerobic conditions during 2, 6 and 24 h in ruminal and abomasal contents collected from untreated adult sheep. Drug concentrations were measured by high-performance liquid chromatography with fluorescence detection after sample clean up and solid phase extraction. Neither MXD nor IVM suffered metabolic conversion and/or chemical degradation after 24-h incubation in ruminal and abomasal contents collected from adult sheep. Unchanged MXD and IVM parent compounds represented between 95.5 and 100% of the total drug recovered in the ruminal and abomasal incubation mixtures compared with those measured in inactive control incubations. The partition of both molecules between the solid and fluid phases of both sheep digestive contents was assessed. MXD and IVM were extensively bound (>90%) to the solid material of both ruminal and abomasal contents collected from sheep fed on lucerne hay. The results reported here confirm the extensive degree of association to the solid digestive material and demonstrates a high chemical stability without evident metabolism and/or degradation for both MXD and IVM in ruminal and abomasal contents. [source] Application of functional group modified substrate in room-temperature phosphorescence, I,, -cyclodextrin modified paper substrate for enrichment and determination of fluorene and acenaphtheneLUMINESCENCE: THE JOURNAL OF BIOLOGICAL AND CHEMICAL LUMINESCENCE, Issue 4-5 2005Ruohua Zhu Abstract A novel method for the determination of fluorene and acenaphthene on solid phase extraction,room-temperature phosphorescence (SPE,RTP) was studied. , -cyclodextrin (, -CD) was chemically bonded onto chromatography paper by reaction with epichorohydrin in an ultrasonic bath. The RTP signal of fluorene and acenaphthene included on the , -CD-modified paper was increased more than 10 times compared with non-modified filter paper, indicating the formation of the inclusion complex. The conditions for the of RTP of compounds were studied in detail. The linear ranges of fluorene and acenaphthene concentrations to the RTP intensity were over two orders of magnitude (8.0 × 10,7,4.0 × 10,5 mol/L for fluorene) with a correlation coefficient of 0.999. The concentration limits of detection for fluorene and acenaphthene were 1.11 × 10,8 mol/L and 3.8 × 10,7 mo/L, respectively. When the sampling volume was 10 µL, the absolute LODs for fluorene and acenaphthene were 18.4 pg/spot and 0.58 ng/spot, respectively. The modified filter paper was used for solid phase extraction (SPE) and the retention behaviour of fluorene and acenaphthene was examined. The enrichment efficiency of the analytes was higher than 100-fold. The SPE,RTP coupling technique was applied directly to the determination of fluorene and acenaphthnene in environmental water samples. Copyright © 2005 John Wiley & Sons, Ltd. [source] Important roles of the hyphenated HPLC-DAD-MS-SPE-NMR technique in metabonomicsMAGNETIC RESONANCE IN CHEMISTRY, Issue S1 2009Huiru Tang Abstract Metabolite identification is a key step for metabonomics study. A fully automated hyphenation of HPLC-diode-array detector (DAD) mass spectrometry (MS) solid phase extraction (SPE),NMR spectroscopy (HPLC-DAD-MS-SPE-NMR) is one of the most efficient methods to determine the structure of a given unknown metabolite in a complex mixture (metabonome) and hence represents one of the most important analytical techniques for the further development of metabonomics. In this review, some recent applications of this technique in identifying novel and trace metabolites in plant extracts and drug metabolism have been discussed. Modification of this hyphenated technique, enabling multiple trappings of strong polar metabolites for biofluids, needs further development. Copyright © 2009 John Wiley & Sons, Ltd. [source] | ||||||||||||||||||||||||||||