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Light Scattering Detector (light + scattering_detector)
Kinds of Light Scattering Detector Selected AbstractsControlled radical polymerization of a trialkylsilyl methacrylate by reversible addition,fragmentation chain transfer polymerizationJOURNAL OF POLYMER SCIENCE (IN TWO SECTIONS), Issue 22 2005M. N. Nguyen Abstract The reversible addition,fragmentation chain transfer (RAFT) polymerization of a hydrolyzable monomer (tert -butyldimethylsilyl methacrylate) with cumyl dithiobenzoate and 2-cyanoprop-2-yl dithiobenzoate as chain-transfer agents was studied in toluene solutions at 70 °C. The resulting homopolymers had low polydispersity (polydispersity index < 1.3) up to 96% monomer conversion with molecular weights at high conversions close to the theoretical prediction. The profiles of the number-average molecular weight versus the conversion revealed controlled polymerization features with chain-transfer constants expected between 1.0 and 10. A series of poly(tert -butyldimethylsilyl methacrylate)s were synthesized over the molecular weight range of 1.0 × 104 to 3.0 × 104, as determined by size exclusion chromatography. As strong differences of hydrodynamic volumes in tetrahydrofuran between poly(methyl methacrylate), polystyrene standards, and poly(tert -butyldimethylsilyl methacrylate) were observed, true molecular weights were obtained from a light scattering detector equipped in a triple-detector size exclusion chromatograph. The Mark,Houwink,Sakurada parameters for poly(tert -butyldimethylsilyl methacrylate) were assessed to obtain directly true molecular weight values from size exclusion chromatography with universal calibration. In addition, a RAFT agent efficiency above 94% was confirmed at high conversions by both light scattering detection and 1H NMR spectroscopy. © 2005 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 43: 5680,5689, 2005 [source] Synthesis and characterization of 2,2-bis(methylol)propionic acid dendrimers with different cores and terminal groupsJOURNAL OF POLYMER SCIENCE (IN TWO SECTIONS), Issue 7 2004Michael Malkoch Abstract Three sets of aliphatic polyester dendrimers based on 2,2-bis(methylol)propionic acid (bis-MPA) were synthesized. Two of the sets had benzylidene terminal groups and either a trimethylolpropane or triphenolic core moiety. The last set had acetonide terminal groups and a triphenolic core moiety. Benzylidene-[G#1]-anhydride and acetonide-[G#1]-anhydride were used as the reactive building blocks in the construction of all dendrimers. The large excess of building blocks used in the coupling reactions initially resulted in considerable material loss. This waste was eliminated through the development of a recycling method. 1H and 13C NMR and matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) analysis were used to verify the purity of all compounds. Size exclusion chromatography (SEC) was used, as well as MALDI-TOF, for molecular weight determinations. The SEC measurements were conducted with a universal calibration method and an online right-angle laser light scattering detector. Measured dendrimer molecular weights were close to their theoretical molar masses. Observations were also made of the hydrodynamic radius and intrinsic viscosity for the different dendrimers. © 2004 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 42: 1758,1767, 2004 [source] Monitoring of mutarotation of monosaccharides by hydrophilic interaction chromatographyJOURNAL OF SEPARATION SCIENCE, JSS, Issue 6-7 2010í Pazourek Abstract Calibration based on the "single-point calibration method", a simple exponential transformation of the response function of an evaporative light scattering detector was improved and applied to analysis of selected saccharides under hydrophilic interaction chromatography mode (a polar phase LiChrospher100 DIOL, mobile phase acetonitrile/water). The improved approach to the calibration procedure yielded a calibration curve with an excellent linearity (quality coefficient <5%). This quantitative evaluation of chromatograms of D -galactose suggested that not only anomers but even pyranose and furanose forms of the anomers could be resolved , the resulting calculations of abundance of the anomeric form strongly correlated with data from the literature obtained mostly by NMR studies (analogous results were also obtained for D -arabinose, D -glucose, and D -mannose). Because of the rapid separation (retention time less than 10,min), the observed correlation enabled to monitor anomeric conversion (mutarotation) of monosaccharides. [source] Silica-based monolithic column with evaporative light scattering detector for HPLC analysis of bacosides and apigenin in Bacopa monnieriJOURNAL OF SEPARATION SCIENCE, JSS, Issue 15-16 2009Pamita Bhandari Abstract A high performance liquid chromatographic method using a silica-based monolithic column coupled with evaporative light scattering detector (HPLC,ELSD) was developed and validated for simultaneous quantification of bacosides (bacoside A, bacopaside I, bacoside A3, bacopaside II, bacopaside X, bacopasaponin C) and apigenin in Bacopa monnieri. The chromatographic resolution was achieved on a Chromolith RP-18 (100×4.6 mm) column with acetonitrile/water (30:70) as mobile phase in isocratic elution at a flow rate of 0.7 mL/min. The drift tube temperature of the ELSD was set to 95°C, and the nitrogen flow rate was 2.0 SLM (standard liter per minute). The calibration curves revealed a good linear relationship (r2 >0.9988) within the test ranges. The detection limits (S/N = 3) and the quantification limits (S/N = 10) for the compounds were in the range of 0.54,6.06 and 1.61,18.78 ,g/mL, respectively. Satisfactory average recovery was observed in the range of 95.8,99.0%. The method showed good reproducibility for the quantification of these compounds in B. monnieri with intra- and inter-day precision of less than 0.69 and 0.67%, respectively. The validated method was successfully applied to quantify analytes in nine accessions of B. monnieri and thus provides a new basis for overall quality assessment of B. monnieri. [source] Asymmetrical flow field-flow fractionation coupled to multiangle laser light scattering detector: Optimization of crossflow rate, carrier characteristics, and injected mass in alginate separationJOURNAL OF SEPARATION SCIENCE, JSS, Issue 14 2007Enrica Alasonati Abstract The coupling of the flow field-flow fractionation (FlFFF) to differential refractive index (DRI) and multiangle laser light scattering (LS) detectors is a powerful tool for characterizing charged polysaccharides such as alginate. However, the correct interpretation of the experimental results and extrapolation of meaningful molecular parameters by using an analytical tool with such a level of complexity requires improvement of the knowledge of the alginate behavior in the channel and careful optimization of the operating conditions. Therefore, the influence of the critical operating parameters, such as crossflow rate, carrier composition and concentration, and sample load, on the alginate retention was carefully evaluated. Combined information obtained simultaneously by DRI and LS detectors over the wide range of the crossflow rate, carrier liquid concentration, and injected amount, allowed to set the appropriate combination of optimal parameters. It was found that the crossflow rate of 0.25 mL/min, carrier solution containing 5×10,2 mol/L ammonium or sodium chloride, and 50,100 ,g of injected sample mass were necessary to achieve complete separation and determination of the meaningful molecular characteristics. The values of the weight-average hydrodynamic radius (RHw), radius of gyration (RG), and molar mass (M), obtained under the optimal conditions were in good agreement to those found for alginates in the literature. [source] Use of evaporative light scattering detector in the detection and quantification of enantiomeric mixtures by HPLCJOURNAL OF SEPARATION SCIENCE, JSS, Issue 10 2006Tong Zhang Abstract Routinely used in our laboratories at analytical scale, an evaporative light scattering detector (ELSD) has proved to be versatile in the detection of enantiomeric resolution using chiral stationary phases by HPLC. Though this kind of detector has been widely used in various domains, its application in enantiomeric resolution has not been discussed in the literature and is found to have very specific features especially in the quantitative perspective. In contrast with the UV detection, the peak area from ELSD for both enantiomers of a racemic mixture may not be the same. This complicates the assessment of the enantiomeric purity of unknown samples. This current work deals with some practical aspects in the detection of enantiomers and in accurate quantitative determination of enantiomeric purity by ELSD. Effects of analyte nature (more precisely molecular weight and volatility), peak shape and peak shape difference between enantiomers on the quantitative integration by ELSD are discussed in connection with the UV-detection results. The calibration for quantitative enantiomeric analysis and its effectiveness are demonstrated. [source] Simple and rapid determination of 1-deoxynojirimycin in mulberry leavesBIOFACTORS, Issue 1-4 2004Toshiyuki Kimura Abstract A simple and rapid method for determining 1-deoxynojirimycin (DNJ), a potent glucosidase inihibitor present in mulberry leaves (Morus alba and Morus bombysis), by high performance liquid chromatography coupled to an evaporative light scattering detector (ELSD) has been developed. DNJ was separated from extract of mulberry leaves on TSK gel Amide-80 column, which is a representative column for hydrophilic interaction chromatography. During post column detection, DNJ was detected by ELSD and concurrently identified by mass spectrometry. The detection limit was 100 ng. This method is sufficiently sensitive for determining DNJ in mulberry leaves and other related products. [source] Quantitative Analysis of Indigo and Indigo Precursors in Leaves of Isatis spp. and Polygonum tinctoriumBIOTECHNOLOGY PROGRESS, Issue 4 2004Kerry G. Gilbert Analysis of extracts from two woad species (Isatis tinctoria and Isatisindigotica) and Polygonum tinctorium revealed that only one indigo precursor (indican) was present in Polygonum, but two precursors were found in Isatis spp. This was done using high performance liquid chromatography (HPLC), coupled to an evaporative light scattering detector (ELSD). In Isatis spp., the indigo precursors indican and a fraction representing isatan B were identified. The proportion of indican and isatan B was different between the two Isatis spp. tested. For the first time, it was possible to quantify the precursors in woad plant species, and the results were found to be in good agreement with those made from total indigo quantification using two different spectrophotometric methods or a derivatization technique. [source] A New HPLC-ELSD Method To Quantify Indican in Polygonum tinctorium L. and To Evaluate ,-Glucosidase Hydrolysis of Indican for Indigo ProductionBIOTECHNOLOGY PROGRESS, Issue 6 2003Luciana G. Angelini A method to quantify the indigo precursor indican (indoxyl-,- d -glucoside) in Polygonum tinctoriumL. has been developed. Plant material was extracted in deionized water, and indican was identified and quantified using high performance liquid chromatography (HPLC) coupled to an evaporative light scattering detector (ELSD). Results confirmed that with this method it is possible to measure indican content in a short time, obtaining reliable and reproducible data. Using this method, leaf indican content was quantified every 15 days during the growing season (from May to October) in P. tinctorium crops grown in a field experiment in Central Italy. Results showed that indican increased along the growing season until flowering and was positively affected by photosynthetic active radiation (PAR). Indican is naturally hydrolyzed by native ,-glucosidase to indoxyl and glucose, the indoxyl yielding indigo. The activity of two enzymes, sweet almond ,-glucosidase and Novarom G preparation, were compared with P. tinctorium native ,-glucosidase to evaluate indigo production. Results showed that the ability to promote indigo formation increased as follows: almond ,-glucosidase , Novarom G. [source] Synthesis of poly(n -hexyl isocyanate- b - N -vinylpyrrolidone) block copolymers by the combination of anionic and nitroxide-mediated radical polymerizations: Micellization properties in aqueous solutionsJOURNAL OF POLYMER SCIENCE (IN TWO SECTIONS), Issue 19 2006Panayiotis Bilalis Abstract A combination of anionic and nitroxide-mediated radical polymerizations (dual initiator) was employed for the synthesis of poly(n -hexyl isocyanate- b - N -vinylpyrrolidone) (PHIC- b -PNVP) block copolymers. The samples were characterized with a size exclusion chromatograph equipped with refractive-index and light scattering detectors as well as 1H NMR spectroscopy. Relatively good control over the molecular weights was achieved. However, rather broad molecular weight distributions were obtained. The micellar properties of the PHIC- b -PNVP block copolymers were studied in water, which is a selective solvent for the poly(N -vinylpyrrolidone) blocks. Static and dynamic light scattering revealed the presence of equilibrium between the micelles and clusters. The clusters partially deaggregated with increasing temperature. © 2006 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 44: 5719,5728, 2006 [source] Simultaneous determination of iridoids, phenolic acids, flavonoids, and saponins in Flos Lonicerae and Flos Lonicerae Japonicae by HPLC-DAD-ELSD coupled with principal component analysisJOURNAL OF SEPARATION SCIENCE, JSS, Issue 18 2007Chun-Yun Chen Abstract A method, HPLC coupled with diode-array and evaporative light scattering detectors (HPLC-DAD-ELSD), was newly developed to evaluate the quality of Flos Lonicerae (FL) and Flos Lonicerae Japonicae (FLJ), through a simultaneous determination of multiple types of bioactive components. By employing DAD, the detection wavelengths were set at 240 nm for the determination of iridoids, 330 nm for phenolic acids, and 360 nm for flavonoids, respectively. While ELSD, connected in series after DAD, was applied to the determination of saponins. This assay was fully validated with respect to precision, repeatability, and accuracy. Moreover, principal component analysis (PCA) was used for the similarity evaluation of different samples, and it was proven straightforward and reliable to differentiate FL and FLJ samples from different origins. For PCA, two principal components have been extracted. Principal component 1 (PC1) influences the separation between different sample sets, capturing 54.598% variance, while principal component 2 (PC2) affects differentiation within sample sets, capturing 12.579% variance. In conclusion, simultaneous quantification of bioactive components by HPLC-DAD-ELSD coupled with PCA would be a well-acceptable strategy to differentiate the sources and to comprehensively control the quality of the medicinal plants FL and FLJ. [source] Determination of seventeen main flavonoids and saponins in the medicinal plant Huang-qi (Radix Astragali) by HPLC-DAD-ELSDJOURNAL OF SEPARATION SCIENCE, JSS, Issue 9 2007Qing-Tao Yu Abstract A simple, rapid, and reliable method, namely high-performance liquid chromatography coupled with diode array and evaporative light scattering detectors (HPLC-DAD-ELSD), was developed to simultaneously determine twelve major flavonoids and five main saponins in different parts of the medicinal plant Huang-qi (Radix Astragali). The DAD wavelength was set at 280 nm for the UV detection of flavonoids, while the drift tube temperature was set at 105°C and the nebulizing gas flow rate at 2.7 L/min for ELSD detection of saponins. The method was fully validated with respect to linearity (r2 >0.998), sensitivity, precision, and accuracy (recovery rate between 93.3 and 104.2%). The analytical results of different parts of the medicinal plant Huang-qi revealed that the levels of total flavonoids or saponins in individual parts can vary considerably and the concentration of each compound in different parts is also significantly different. The aerial parts (stems and leaves) contain even higher total contents of flavonoids (although of different kinds) than the commonly used roots of the plants. In addition, the concentration of total flavonoids and saponins in the extract of the fibrous roots was surprisingly highest among all parts of Astragalus species. All of these findings provide clear evidence and scientific support for utilization of different parts of the medicinal plant Huang-qi and also for reduction in waste of plant resources. [source] Simultaneous determination of twelve bioactive constituents in Buyang Huanwu decoction by HPLC-DAD-ELSD and HPLC-TOF/MSBIOMEDICAL CHROMATOGRAPHY, Issue 2 2010E-Hu Liu Abstract Buyang Huanwu Decoction (BYHYD) is a classical traditional Chinese medicinal prescription that has been widely used for treating cerebrovascular illnesses for hundreds of years. In this study, a comprehensive analytical method has been developed for quantitative analysis of the major constituents in BYHWD. This method was based on high-performance liquid chromatography coupled to a diode array and evaporative light scattering detectors (HPLC-DAD-ELSD) on a common reverse-phase C18 column. HPLC coupled with on-line time-of-flight mass spectrometry (HPLC-TOF/MS) was additionally adopted to provide further validation for the constituents. It was found that 0.3% aqueous formic acid and acetonitrile was the optimum mobile phase for gradient elution. This method, which showed excellent precision and accuracy, was successfully applied to quantify the bioactive constituents in six BYHWD products. The validated HPLC-DAD-ELSD method, together with the HPLC-TOF/MS analysis, provided a new basis for assessing the quality of traditional Chinese medicinal prescription consisting of many bioactive components. Copyright © 2009 John Wiley & Sons, Ltd. [source] Heating-induced conformational change of a novel ,-(1,3)- D -glucan from Pleurotus geestanusBIOPOLYMERS, Issue 2 2010Mei Zhang Abstract Recently, we isolated and purified a neutral polysaccharide (PGN) from edible fungus Pleurotus geestanus. Its structure was characterized by a range of physical,chemical methods, including high performance anion exchange chromatography, uronic acid, and protein analyses, size exclusion chromatography with ultraviolet, refractive index and light scattering detectors, and nuclear magnetic resonance. Our results revealed that PGN is a novel ,-(1,3)- D -glucan with glucose attached to every other sugar residues at Position 6 in the backbone. It has a degree of branching of 1/2. Such structure is different from typical ,-(1,3)- D -glucans schizophyllan and lentinan in which DB is 1/3 and 2/5, respectively. Rheological study showed a very interesting melting behavior of PGN in water solution: heating PGN in water leads to two transitions, in the range of 8,12.5°C and 25,60°C, respectively. The melting behavior and conformational changes were characterized by rheometry, micro-differential scan calorimetry, atomic force microscopy, static and dynamic light scattering at different temperatures. The first heating-induced transition corresponds to the disintegration of polymer bundles into small helical clusters, resembling the heating-induced dissociation of SPG in water at 7°C; the second one might correspond to the dissociation of helical strands to individual chains. The ability of PGN to undergo a conformation/viscosity transition in water upon heating is very valuable to immobilize cells or enzymes or therapeutic DNA/RNA, which makes PGN a potentially useful biomaterial. © 2009 Wiley Periodicals, Inc. Biopolymers 93: 121,131, 2010. This article was originally published online as an accepted preprint. The "Published Online" date corresponds to the preprint version. You can request a copy of the preprint by emailing the Biopolymers editorial office at biopolymers@wiley.com [source] | |||||||||||||