Search results for "LIMIT"
showing 10 items of 2826 documents
Direct ATR-FTIR determination of sucrose in beet root.
2000
A simple and fast procedure has been developed for the direct determination of sucrose in beet root samples through attenuated total reflectance Fourier transform infrared absorbance measurements (ATR-FTIR) at 1056 cm(-1) with a baseline established between 1187 and 887 cm(-1). The method only requires a previous crushing or liquefaction of samples and it is free from matrix effects and from the interference of minoritary sugars and fermentation molecules. Aqueous solutions of sucrose can be used as standards and recovery values from 101 to 103% were found for spiked concentration levels from 3.5 to 10.5% (w/w). The limit of detection provided by this method corresponds to 0.15% (w/w) of su…
PLS-NIR determination of total sugar, glucose, fructose and sucrose in aqueous solutions of fruit juices
1997
Abstract An analytical procedure has been developed for the direct determination of sugars in fruit juice samples. The method is based on the partial least-squares (PLS) treatment of first derivative near infrared (NIR) spectroscopic data obtained between 1200 and 2450 nm, using 1 mm pathlength cell and a multicomponent calibration set, including seven binary mixtures and 10 ternary mixtures of glucose, fructose and sucrose. The limit of detection values found are of the order of 0.2 g/100 ml for total sugar and 0.2, 0.4 and 0.5 g/100 ml for glucose, fructose and sucrose, respectively. Relative standard deviation values obtained vary from 0.4% to 2.3% for six independent measurements of ind…
Quantification of low levels of amorphous content in sucrose by hyperDSC.
2005
A method was developed for the quantification of low levels of amorphous content in sucrose with hyperDSC. The method was based on the fact that the change of specific heat at the glass transition is linearly proportional to the amorphous content. It was found out that as annealing time increased, the glass transition temperature moved to a higher temperature and the change of specific heat increased. DeltaC(p) for annealed totally amorphous sucrose was 0.761+/-0.012 Jg(-1) degrees C(-1). Synthetic mixtures with various proportions of crystalline and amorphous sucrose were prepared. The following linear regression between DeltaC(p) and amorphous content was obtained: DeltaC(p)=0.0075x - 0.0…
Determination of sulphonamides in human urine by azo dye precolumn derivatization and micellar liquid chromatography
1995
Abstract A high-performance liquid chromatographic method for the determination of sulphonamides in urine is reported. The drugs (sulphadiazine, sulphaguanidine, sulphamethizole, sulphamethoxazole, and sulphathiazole) were diazotized with nitrite and coupled with N-(1-naphthyl)ethylenediamine dihydrochloride in a sodium dodecyl sulphate (SDS) micellar medium. Separation of the sulphonamide azo dyes was performed on a C18 column with a 0.05 M SDS-2.4% pentanol mobile phase, which permitted the direct injection of the urine samples. The limits of detection were in the 0.1–0.3 μg/ml range.
Identification of the Biotransformation Products of 2-Ethylhexyl 4-(N,N-Dimethylamino)benzoate
2010
Nowadays, 2-ethylhexyl 4-(N,N-dimethylamino)benzoate (EDP) is one of the most widely used UV filters in sunscreen cosmetics and other cosmetic products. However, undesirable processes such as percutaneous absorption and biological activity have been attributed to this compound. The in vitro metabolism of EDP was elucidated in the present work. First of all, the phase I biotransformation was studied in rat liver microsomes and two metabolites, N,N-dimethyl-p-aminobenzoic acid (DMP) and N-monomethyl-p-aminobenzoic acid (MMP), were identified by GC-MS analysis. Secondly, the phase II metabolism was investigated by means of LC-MS. The investigated reactions were acetylation and glucuronidation …
Fast extraction of cannabinoids in marijuana samples by using hard-cap espresso machines
2018
Abstract A simple, quick and low cost procedure was developed for the extraction of Δ9-tetrahydrocannabinol, cannabidiol, and cannabinol from marijuana samples, based on the use of a hard-cap espresso extraction with 2-propanol. After extraction, cannabinoids were directly determined after appropriate dilution by gas-chromatography-mass spectrometry, reaching a limit of detection from 0.03 to 0.05 mg g−1. Extraction efficiency was evaluated by the comparison of results obtained for seized samples by the proposed method and a reference methodology based on ultrasound-assisted extraction. Moreover, ion mobility was proposed for the rapid and sensitive determination of Δ9-tetrahydrocannabinol …
Multicommutation as an environmentally friendly analytical tool in the hydride generation atomic fluorescence determination of tellurium in milk.
2003
The aim of this study is to show the advantages of the emerging multicommutation methodology based on the use of solenoid valves for Te determination in milk by hydride generation atomic fluorescence spectrometry (HG-AFS). The delivery of a series of alternating sequential insertions of small volumes of samples and reagents gives rise to new hydrodynamic processes and exciting analytical potentials by controlling the time of flow through the on/off-switched solenoid valves. This drastically reduces the reagent consumption by a factor of 4 and the generation of effluents (590 mL h(-1) instead of 750 mL h(-1) generated by the continuous-mode measurement) and also provides an improvement in th…
Simple and sensitive reversed-phase liquid chromatographic assay for analysis of chlorthalidone in urine
1993
Abstract This study describes a rapid method for the determination of chlorthalidone in human urine by reversed-phase liquid chromatography and UV detection at 230 nm, after clean-up over a C8 solid-phase extraction column. Liquid chromatography was carried out on a C18-bonded phase using acetonitrile-phosphate buffer (pH=3) gradient elution. Triamterene was used as internal standard. The system has been applied to the determination of chlorthalidone in the 0.10–10.0 μg/mL concentration interval; the limit of detection was 6 ng/mL.
Comparison of different sorbents for on-line liquid-solid extraction followed by high-performance liquid chromatographic determination of nitrogen-co…
1998
Abstract LiChrolut EN [poly(styrene-divinylbenzene), PSDVB], Carbograph (graphitized carbon black, GCB), Isolute CN (cyanopropylsilica), Isolute C 2 (ethylsilica), and LiChrospher RP18 (octadecylsilica) were studied for on-line solid-phase extraction of twelve nitrogen containing pesticides from water. Determination (UV 210 nm) was performed with a Spherisorb C 8 analytical column and an acetonitrile-water gradient. The mean recoveries from 50 ml ranged from 83% for RP18 to 44% for GCB, and decreased in the following order: RP18, CN, LiChrolut EN, C 2 , and GCB. GCB showed poor recoveries due to incomplete desorption with the acetonitrile-water gradient used, and memory effects were detecte…
Bio-metal-organic frameworks for molecular recognition and sorbent extraction of hydrophilic vitamins followed by their determination using HPLC-UV
2020
A bio-metal-organic framework (bio-MOF) derived from the amino acid L-serine has been prepared in bulk form and evaluated as sorbent for the molecular recognition and extraction of B-vitamins. The functional pores of bio-MOF exhibit high amounts of hydroxyl groups jointly directing other supramolecular host-guest interactions thus providing the recognition of B-vitamins in fruit juices and energy drinks. Single-crystal X-ray diffraction studies reveal the specific B-vitamin binding sites and the existence of multiple hydrogen bonds between these target molecules and the framework. It offered unique snapshots to accomplish an efficient capture of these solutes in complex aqueous matrices. Fo…