Flow systems exploiting in-line prior assays

An expert sequential injection system involving a prior assay is proposed for spectrophotometric determination of phosphate and eventually zinc in soil extracts. The result of phosphate determination is the basis for a concentration-oriented decision regarding to the need or not for zinc determination. Zinc was only determined if a threshold value (peak height corresponding to 5.0 mg l⁻¹ P) was surpassed. The methods involved formation of molybdenum blue and the Rhodamine 6G/ammonium thiocyanate/Zn²⁺ ternary complex. Variations in the threshold value were < 2% during 4 h operating periods, false responses were not verified, and the analytical time was reduced in about 30%. Precise results (R.S.D. <3% P and < 1% Zn) in agreement with spectrophotometry and flame atomic absorption spectrometry were obtained. The innovation permits faster information processing, as well as a reduction in the number of measurements, number of analytical steps, laboratorial time, and consumption of sample and reagents, thus waste generation.     

Preparation of β-hydroxyesters from isoxazolines. A selective Nibpy-catalyzed electrochemical method

An electrocatalytic method for the reductive N-O cleavage of isoxazolines is described. Ni⁰bpy, generated in situ, was used to promote selective ring opening of 3-methoxy-5-phenylisoxazoline (1a) and 3-methoxy-[4,5]cyclohexylisoxazoline (1b). DMF and NaI were used as solvent and supporting electrolyte, and β-hydroxyesters 2a and 2b were obtained in high yields respectively, after acid hydrolysis. β-Hydroxynitriles 3a and 3b were also identified as side products.     

Sharp determinants

We introduce a sharp trace Tr^# and a sharp determinant Det^#(1-z) for an algebra of operators acting on functions of bounded variation on the real line. We show that the zeroes of the sharp determinant describe the discrete spectrum of . The relationship with weighted zeta functions of interval maps and Milnor-Thurston kneading determinants is explained. This yields a result on convergence of the discrete spectrum of approximated operators.Oblatum 8-V-1995 & IX-1995On leave from CNRS, UMR 128, ENS Lyon, France     

A New ent‐Kaurane Diterpene from Stems of Alibertia macrophylla K. Schum. (Rubiaceae)

Phytochemical investigations of the stems of a specimen of Alibertia macrophylla led to the isolation and characterization of the new diterpene ent‐kaurane‐2β,3α,16α‐triol ( 1 ), along with triterpenes 2 – 8 , iridoids 9 – 12 , and phenolic acids 13 – 15 . The structure of 1 was established based on spectroscopic studies (¹H‐ and ¹³C‐NMR, IR, and HR‐ESI‐MS). This is the first report of the isolation of a diterpene from the Alibertia genus in Rubiaceae.     

Quantitative analysis of delta9-tetrahydrocannabinol in preserved oral fluid by liquid chromatography-tandem mass spectrometry

A rapid and sensitive method for the analysis of delta9-tetrahydrocannabinol (THC) in preserved oral fluid was developed and fully validated. Oral fluid was collected with the Intercept, a Food and Drug Administration (FDA) approved sampling device that is used on a large scale in the U.S. for workplace drug testing. The method comprised a simple liquid-liquid extraction with hexane, followed by liquid chromatography-tandem mass spectrometry (LC-MS-MS) analysis. Chromatographic separation was achieved using a XTerra MS C18 column, eluted isocratically with 1 mM ammonium formate-methanol (10:90, v/v). Selectivity of the method was achieved by a combination of retention time, and two precursor-product ion transitions. The use of the liquid-liquid extraction was demonstrated to be highly effective and led to significant decreases in the interferences present in the matrix. Validation of the method was performed using both 100 and 500 MicroL of oral fluid. The method was linear over the range investigated (0.5-100 ng/mL and 0. 1-10 ng/mL when 100 and 500 microL, respectively, of oral fluid were used) with an excellent intra-assay and inter-assay precision (relative standard deviations, RSD <6%) for quality control samples spiked at a concentration of 2.5 and 25 ng/mL and 0.5 and 2.5 ng/mL, respectively. Limits of quantification were 0.5 and 0.1 ng/mL when using 100 and 500 microL, respectively. In contrast to existing GC-MS methods, no extensive sample clean-up and time-consuming derivatisation steps were needed. The method was subsequently applied to Intercept samples collected at the roadside and collected during a controlled study with cannabis.     

Low-temperature exfoliation of multilayer-graphene material from FeCl3 and CH3NO2 co-intercalated graphite compound

Microwave induced rapid decomposition of nitromethane at low temperature exfoliates the graphene sheets from the FeCl(3) and CH(3)NO(2) co-intercalated graphite compound without creating many defects and functional groups. This approach provides a scalable method for high-quality graphene materials via low-temperature exfoliation of graphite under mild chemical conditions.     

Synthesis,structural characterization and reactivity of copper(I)-nitrile complexes: Crystal and molecular structure of [Cu(BzCN)4][BF4]

Complexes of general formula [CuL₄][BF₄] (L = benzonitrile – PhCN 2 or phenylacetonitrile – BzCN 3) have been prepared and structurally characterized by NMR spectroscopy and X-ray crystallography. Their structure and reactivity have been compared to the well known [Cu(MeCN)₄][BF₄] (1). The ⁶³Cu line width and the ⁶³Cu chemical shift have been evaluated by varying the temperature and the concentration of the complex 2 in benzonitrile solutions. The phenylacetonitrile solutions of the complex 3 give extremely broad signals which are beyond detection. Accordingly, compound 3 has been studied by ⁶³Cu MAS NMR spectroscopy. The solution NMR data are consistent to the prevalence of dynamic equilibrium between tetra- and low-coordinated species in both complexes. The X-ray structure of 3 revealed that the copper(I) atom sits in a slightly distorted tetrahedral geometry, surrounded by four BzCN ligands.     

Implementation of an integrated glucose POCT system

In response to a change of the Belgian National Directives whereby hospital laboratories became responsible for all point-of-care testing (POCT) performed within hospital walls a standardized and automated POC glucose-testing system was implemented in our hospital. The system consists of 50 AccuCheck Inform instruments (Roche Diagnostics, Vilvoorde, Belgium), 50 docking stations, a DataCare Server, and connections to the medical laboratory information system (MOLIS, Sysmex, Barchon, Belgium) and to the hospital information system. Implementation involved many parties and extensive preparation and communication. Key issues were bar-coded patient and user identification, training, and responsibilities. One year after the hospital wide implementation of this system the quality of POC glucose testing has significantly increased, thereby improving patient safety. This study describes a stepwise change over involving the medical laboratory and with a focus on hands-on quality.Presented at the ninth conference on Quality in the Spotlight, 18–19 March 2004, Antwerp, Belgium.