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1.
Solution-enhanced dispersion by supercritical fluids (SEDS) was applied to produce nano-sized recombinant human growth hormone
(hGH) particles. Ethanol was used to help the supercritical carbon dioxide to extract water from the aqueous protein solution.
Various sizes of hGH nanoparticles were successfully prepared with a narrow particle size distribution from aqueous ethanol
solution without using any additive. The theoretical particle sizes were deduced from the calculated droplet sizes based on
a modified Jasuja’s equation. The calculated mean particle sizes and the experimentally obtained ones were compared and the
results showed an excellent correlation coefficient (R
2) of 0.995.
Figure Distribution of hGH Nano-particles 相似文献
2.
Determining sulfamonomethoxine and its acetyl/hydroxyl metabolites in chicken plasma under organic solvent-free conditions 总被引:1,自引:0,他引:1
Furusawa N 《Analytical and bioanalytical chemistry》2006,385(8):1570-1574
A quantitative technique is described for a sample preparation followed by high performance liquid chromatography method for
the simultaneous determination of sulfamonomethoxine and its metabolites, N
4-acetyl SMM and 2,6-dihydroxy SMM, in chicken plasma. The average recoveries, analytical total time, and limits of quantitation
were ≥80% (relative standard deviations (SD) ≤6%), <30 min sample-1 (12 samples in 2 h), and ≤0.09 μg ml−1, respectively. The procedure, performed under 100% aqueous conditions, uses no organic solvents and toxic reagents at all
and is, therefore, harmless to the environment and humans.
相似文献
3.
Lee KC Cheuk MW Chan W Lee AW Zhao ZZ Jiang ZH Cai Z 《Analytical and bioanalytical chemistry》2006,386(7-8):2225-2232
A reversed-phase HPLC method has been developed for determination of twelve intact glucosinolates—glucoiberin, glucocheirolin,
progoitrin, sinigrin, epiprogoitrin, glucoraphenin, sinalbin, gluconapin, glucosibarin, glucotropaeolin, glucoerucin, and
gluconasturtiin—in ten traditional Chinese plants. The samples were extracted with methanol and the extracts were cleaned
on an activated Florisil column. A mobile phase gradient prepared from methanol and 30 mmol L−1 ammonium acetate at pH 5.0 enabled baseline separation of the glucosinolates. Glucosinolate detection was confirmed by quadrupole
time-of-flight tandem mass spectrometric analysis in negative-ionization mode. Detection limits ranged from 0.06 to 0.36 μg
g−1 when 5 g of dried plant was analyzed. Recoveries of the glucosinolates were better than 85% and precision (relative standard
derivation, n = 3) ranged from 5.3 to 14.6%. Analysis of the glucosinolates provided scientific evidence enabling differentiation of three
pairs of easily confused plants.
Figure Glucosinolates Analysis for the Differentiation of Easily-Confusing Herbs 相似文献
4.
n-Butyl benzyl phthalate (BBP) is an endocrine-disrupting chemical. A bacterium species capable of using BBP as the sole source
of carbon and energy was isolated from mangrove sediment. Effects of BBP concentration, pH, temperature, and salinity on BBP
biodegradation were studied. The optimum pH, temperature, and salinity for the BBP biodegradation were 7.0, 37°C, and 15 g L−1, respectively. BBP was completely degraded within 6 days under optimum conditions, and the biodegradation of BBP could be
fitted to a first-order kinetic model. The major metabolites of BBP biodegradation were identified as mono-butyl phthalate,
mono-benzyl phthalate, phthalic acid, and benzoic acid by using high-performance liquid chromatography and gas chromatography–mass
spectrometry. A preliminary metabolic pathway was proposed for the biodegradation of BBP.
相似文献
5.
6.
Gerard P. O’Sullivan Norma M. Scully Jean-Marie Prat Jeremy D. Glennon Benjamin Dietrich Volker Friebolin Klaus Albert 《Analytical and bioanalytical chemistry》2009,394(5):1261-1272
Supercritical carbon dioxide has attracted attention as a potential replacement for traditional organic solvents due to its
simplified workup procedures and reduced environmental impact—providing a green chemistry approach for organic solvent-free
functionalisation. In addition to the environmental benefits, the enhanced diffusivity observed in supercritical solvents
can often enhance reaction rates. We have applied these valuable features to the preparation of silica-bonded stationary phases
and examined their potential in liquid chromatography. We report the successful preparation and characterisation of polyether
silica based on Frechet dendrimers—this significantly enhances the range of stationary-phase chemistries that can be prepared
in supercritical fluids. First- and second-generation polyether silicas were prepared, characterised, end-capped and evaluated
for use as stationary phases for liquid chromatography.
Figure SRM1649 on 2nd generation polyether silica
Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users.
相似文献
Jeremy D. GlennonEmail: |
7.
A method based on use of functionalized gold nanoparticles on polyethylenimine film has been developed for colorimetric detection of immunoglobulin G (IgG). The immunogold nanoparticles were immobilized on quartz slides by recognition between antibody and antigen, with the antigen chemically adsorbed on the polyethylenimine film. By measurement of the UV–visible spectra of the immobilized immunogold, detection of h-IgG was achieved. The detection limit for h-IgG by use of this method can be as low as 0.01 μg mL−1. This method is quite promising for numerous applications in immunoassay.
Figure 相似文献
8.
Gergely A Szász G Szentesi A Gyimesi-Forrás K Kökösi J Szegvári D Veress G 《Analytical and bioanalytical chemistry》2006,384(7-8):1506-1510
The biological importance of dehydroepiandrosterone (DHEA) is reflected by the fact that DHEA is a crucial precursor of the biosynthesis of the steroidal sex hormones. Simultaneous separation of DHEA, dehydroepiandrosterone sulfate (DHEA-S), pregnenolone, androstenedione and testosterone has been accomplished by reversed-phase ion-pair high-performance liquid chromatography (RP-IP-HPLC) based on isocratic elution applying circular dichroism (CD) detection at 295 nm. Addition of tetrabutylammonium hydrogensulfate to the mobile phase increases the retention of DHEA-S on the C8-silica column by an apparent ion-pairing mechanism without affecting the retention of the other (non-ionic) steroids. CD spectroscopy provides highly selective detection of compounds possessing optically active absorption bands and the separation is even more selective in the higher wavelength range applied. The linearity of the steroid concentration (c, mg mL−1) versus peak area was tested in the concentration range of 0.5–2 mg mL−1 (injected quantities were 10–40 μg). The relative standard deviation (RSD) values for DHEA and DHEA-S indicated a good intra-assay and inter-assay precision of the method.
相似文献
9.
An X-ray fluorescence method (XRF) is presented that allowed low detection limits (at the 0.1–23 ng mL−1 level) to be obtained for Cr, Mn, Fe, Ni, Zn, Sr, Pb, Bi and Br in water. The samples were prepared using a thin layer method. Trace elements were determined via the calibration curve and standard addition. Absorption effects and inhomogenities in prepared samples were checked for using the emission–transmission method and internal standards, respectively. The results from the XRF method were compared with the results from the inductively coupled plasma atomic emission spectrometry method.
相似文献
10.
Pisonero J Kroslakova I Günther D Latkoczy C 《Analytical and bioanalytical chemistry》2006,386(1):12-20
The spatial distribution and concentration of impurities in metallurgical-grade silicon (MG-Si) samples (97–99% w/w Si) were investigated by use of laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). The spatial resolution
(120 μm) and low limits of detection (mg kg−1) for quality assurance of such materials were studied in detail. The volume-dependent precision and accuracy of non-matrix-matched
calibration for quantification of minor elements, using NIST SRM 610 (silicate standard), indicates that LA-ICP-MS is well
suited to rapid process control of such materials. Quantitative results from LA-ICP-MS were compared with previously reported
literature data obtained by use of ICP-OES and rf-GD-OES. In particular, the distribution of element impurities and their
relationship to their different segregation coefficients in silicon is demonstrated.
Dedicated to Professor Klaus G. Heumann 相似文献
11.
Preparative HPLC separation of bambuterol enantiomers and stereoselective inhibition of human cholinesterases 总被引:2,自引:0,他引:2
Gazić I Bosak A Sinko G Vinković V Kovarik Z 《Analytical and bioanalytical chemistry》2006,385(8):1513-1519
We separated and characterized the enantiomers of bambuterol (5-[-(tert-butylamino)-1-hydroxyethyl]-m-phenylene-bis(dimethylcarbamate) hydrochloride), which is used in racemic form as a prodrug of terbutaline, a β2-adrenoceptor agonist. The enantioseparation was attempted on several chiral HPLC columns, and the most effective separation
was achieved on the amylose-based Chiralpak AD column. Since in vivo conversion of bambuterol into terbutaline involves hydrolysis
by butyrylcholinesterase (EC 3.1.1.8), we studied the reaction of enantiomers with eight human BChE variants. Both enantiomers
inhibited all studied BChE variants; however, the rate of inhibition with the (R)-enantiomer was about five times faster than with the (S)-enantiomer. (R)-bambuterol inhibition rate constants for homozygous usual (UU), fluoride-resistant (FF) or atypical (AA) variant ranged
from 6.4 to 0.11 min-1μM-1. The inhibition rates for heterozygotes were between the respective constants for the corresponding homozygotes.
An erratum to this article can be found at 相似文献
12.
Ruben t’Kindt Andris Jankevics Richard A. Scheltema Liang Zheng David G. Watson Jean-Claude Dujardin Rainer Breitling Graham H. Coombs Saskia Decuypere 《Analytical and bioanalytical chemistry》2010,398(5):2059-2069
Comparative metabolomics of Leishmania species requires the simultaneous identification and quantification of a large number of intracellular metabolites. Here,
we describe the optimisation of a comprehensive metabolite extraction protocol for Leishmania parasites and the subsequent optimisation of the analytical approach, consisting of hydrophilic interaction liquid chromatography
coupled to LTQ-orbitrap mass spectrometry. The final optimised protocol starts with a rapid quenching of parasite cells to
0 °C, followed by a triplicate washing step in phosphate-buffered saline. The intracellular metabolome of 4 × 107 parasites is then extracted in cold chloroform/methanol/water 20/60/20 (v/v/v) for 1 h at 4 °C, resulting in both cell disruption and comprehensive metabolite dissolution. Our developed metabolomics
platform can detect approximately 20% of the predicted Leishmania metabolome in a single experiment in positive and negative ionisation mode.
相似文献
13.
M. Dabiri Ali A. Mohammadi Hassan Qaraat 《Monatshefte für Chemie / Chemical Monthly》2009,140(4):401-404
Abstract An efficient and direct procedure for the synthesis of novel spiro[isoindoline-1,2′-quinazoline]-3,4′(3′H)-dione derivatives is described. The process employs a condensation reaction of 2-aminobenzamides and isatins in the presence
of a catalytic amount of KAl(SO4)2.12H2O (alum) in ethanol under reflux.
Graphical Abstract
相似文献
14.
Zaher M Ravelet C Baussanne I Ravel A Grosset C Décout JL Peyrin E 《Analytical and bioanalytical chemistry》2009,393(2):655-660
In this paper, we describe the preparation and the evaluation of a porous graphitic carbon (PGC) column coated with a new
dinaphthyl derivative of neamine for chiral ligand-exchange (LE) chromatography. It was shown that the graphitic surface/dinaphthyl
anchor system efficiently (1.15 μmol/m2) and stably (three months of intensive use) adsorbs the neamine template onto the chromatographic support. The resulting
coated PGC stationary phase showed appreciable LE-based enantioselective properties towards several native amino acids.
Chromatographic separation of methionine enantiomers using a dinaphtyl neamine-based ligand-exchange chiral stationary phase 相似文献
15.
A new spectrofluorimetric method was developed for the determination of trace amounts of lecithin using the ciprofloxacin (CIP)–terbium (Tb3+) ion complex as a fluorescent probe. In a buffer solution at pH=5.60, lecithin can remarkably reduce the fluorescence intensity of the CIP–Tb3+ complex at λ=545 nm. The reduced fluorescence intensity of the Tb3+ ion is proportional to the concentration of lecithin. Optimum conditions for the determination of lecithin were also investigated. The linear range and detection limit for the determination of lecithin were 1.0×10−6–3.0×10−5 mol L−1 and 3.44×10−7 mol L−1, respectively. This method is simple, practical, and relatively free of interference from coexisting substances. Furthermore, it has been successfully applied to assess lecithin in serum samples.
相似文献
16.
A novel thiocyanate (SCN−)-selective PVC membrane electrode based on a zinc-phthalocyanine (ZnPc) complex as neutral carrier is described. The membrane electrode containing ZnPc with 5.1% (w/w) ionophore, 29.2% (w/w) PVC, and 65.7% (w/w) 2-nitrophenyl octyl ether (o-NPOE) as plasticizer displayed an anti-Hofmeister selectivity sequence , and exhibited near-Nernstian potential response to thiocyanate ranging from about 1.0×10−1 to 1.0×10−6 mol L−1 with a detection limit of 7.5×10−7 mol L−1 and a slope of 58.1±0.5 mV per decade in pH 3.0 phosphate buffer solution at 25 °C. This preferential response is believed to be associated with the unique coordination between the central metal of the carrier and thiocyanate.
相似文献
17.
Herschbach H Hosomizu K Hahn U Leize E Van Dorsselaer A Imahori H Nierengarten JF 《Analytical and bioanalytical chemistry》2006,386(1):46-51
The electrospray mass spectrometric characterization of neutral dendrons with a carboxylic acid function or a t-butyl ester moiety at the central point and up to eight peripheral C60 subunits has been performed and is described in detail. Molecules bearing a carboxylic acid group at the center turned out
to be preferentially ionized by deprotonation, whereas those with a t-butyl ester head group were ionized by reduction of the C60 units in the infusion capillary of the electrospray source.
Electronic supplementary material Supplementary material is available for this article at and is accessible for authorized users. 相似文献
18.
Screening and analysis of an antineoplastic compound in Rhizoma Chuanxiong by means of in vitro metabolism and HPLC-MS 总被引:1,自引:0,他引:1
A new screening and analysis method that combines in vitro metabolism with high-performance liquid chromatography-mass spectrometry
(HPLC-MS) was developed for the screening and analysis of an antineoplastic compound, coniferyl ferulate, which is present
in the rhizome of Rhizoma Chuanxiong. Infrared (IR), ultraviolet visible spectroscopy (UV-Vis), nuclear magnetic resonance (NMR) and element analysis were used
to identify the molecular structure of coniferyl ferulate. The quantitative analysis of coniferyl ferulate in different extracts
of Rhizoma Chuanxiong was carried out, and the metabolism of coniferyl ferulate was investigated by in vitro incubation with rat liver homogenate.
The metabolite of coniferyl ferulate, ferulic acid ethyl ester, was identified by HPLC-MS, UV-Vis and IR. In addition, antineoplastic
activities of coniferyl ferulate and ferulic acid ethyl ester were detected by the MTT assay. The observed inhibition rate
of coniferyl ferulate on the activity of HeLa cells was over 80% at 5.4 ng μl−1. However, its metabolite, ferulic acid ethyl ester, showed no antineoplastic activity in vitro.
相似文献
19.
Analysis of type I and IV collagens by FT-IR spectroscopy and imaging for a molecular investigation of skeletal muscle connective tissue 总被引:2,自引:0,他引:2
Petibois C Gouspillou G Wehbe K Delage JP Déléris G 《Analytical and bioanalytical chemistry》2006,386(7-8):1961-1966
Many muscular diseases result from abnormal organization of connective tissue and/or collagen network formation. Only a few
molecular imaging techniques are able to analyze this collagen network by differentiating collagen types. In this study, FT-IR
spectroscopy was used to analyze type I and IV collagens, the most important compounds of which are perimysium and endomysium,
respectively. Secondary structure of collagen types was determined by curve-fitting the 1,700–1,480 cm−1 spectral interval. Type I collagen could be differentiated from type IV by its higher amounts of triple helix and α-helix,
but lower amounts of β-sheets (P < 0.01). FT-IR imaging was then used to determine structural features of perimysium and endomysium collagen network in bovine
Flexor carpi radialis muscle. Secondary structure of proteins contained in perimysium and endomysium was found to be very close to type I and IV
collagens, respectively. FT-IR spectroscopy and imaging are thus analytical tools that might be used for investigating biodistribution
and assembly of collagen types in connective tissues.
Figure Visible (left) and full spectral FT-IR (right) images of skeletal muscle tissue section (16 μm) exhibiting a vertical arrangement of fibers. + and × in FT-IR image show
selected positions to obtain FT-IR spectra of perimysium and endomysium, respectively 相似文献
20.
C. R. Dockery A. R. Stefan A. A. Nieuwland S. N. Roberson B. M. Baguley J. E. Hendrix S. L. Morgan 《Analytical and bioanalytical chemistry》2009,394(8):2095-2103
Systematic designed experiments were employed to find the optimum conditions for extraction of direct, reactive, and vat dyes
from cotton fibers prior to forensic characterization. Automated microextractions were coupled with measurements of extraction
efficiencies on a microplate reader UV–visible spectrophotometer to enable rapid screening of extraction efficiency as a function
of solvent composition. Solvent extraction conditions were also developed to be compatible with subsequent forensic characterization
of extracted dyes by capillary electrophoresis with UV–visible diode array detection. The capillary electrophoresis electrolyte
successfully used in this work consists of 5 mM ammonium acetate in 40:60 acetonitrile–water at pH 9.3, with the addition
of sodium dithionite reducing agent to facilitate analysis of vat dyes. The ultimate goal of these research efforts is enhanced
discrimination of trace fiber evidence by analysis of extracted dyes.
Figure Fitted absorbance response surface for extraction of a direct dye, C. I. yellow 58, using a ternary solvent system. 相似文献