A comprehensive chromatographic comparison of amphetamine and methylamphetamine extracted from river water using molecular imprinted polymers and without the need for sample derivatization

This work explores the differences between two GCMS instruments for the determination of amphetamine and methylamphetamine extracted from water samples (ultra pure water and river water) without the necessity for derivatization. The instruments contained different generations of gas chromatograph and mass selective detector components and revealed significantly different results when presented with the same samples. The extraction methodology also compared two SPE systems. The extraction efficiency of commercially available molecular imprinted polymers as a sorbent in SPE was compared with commonly used hydrophilic balance sorbent. Molecular imprinted polymers provided excellent recoveries (81 ± 2% and 108 ± 3% at 30 μg L^?1, and 94 ± 2% and 94 ± 2% at 200 μg L^?1 for amphetamine and methylamphetamine, respectively). The best LOD obtained was sufficient for the determination of both drugs extracted from river water (0.029 ± 0.003 and 0.015 ± 0.004 μg L^?1 for amphetamine and methylamphetamine, respectively). These were comparable to literature values obtained through conventional extraction and analysis using LC‐MS/MS but had the advantage of being achieved using an underivatized GCMS method.     

A 3D mammalian cell separator biochip

The dissimilar cytoskeletal architecture in diverse cell types induces a difference in their deformability that presents a viable approach to separate cells in a non-invasive manner. We report on the design and fabrication of a robust and scalable device capable of separating a heterogeneous population of cells with variable degree of deformability into enriched populations with deformability above a certain threshold. The three dimensional device was fabricated in fused silica by femtosecond laser direct writing combined with selective chemical etching. The separator device was evaluated using promyelocytic HL60 cells. Using flow rates as large as 167 μL min(-1), throughputs of up to 2800 cells min(-1) were achieved at the device output. A fluorescence-activated cell sorting (FACS) viability analysis on the cells revealed 81% of the population maintain cellular integrity after passage through the device.     

Rapid distinction of intracellular and extracellular proteins using NMR diffusion measurements

In-cell NMR spectroscopy offers a unique opportunity to begin to investigate the structures, dynamics, and interactions of molecules within their functional environments. An essential aspect of this technique is to define whether observed signals are attributable to intracellular species rather than to components of the extracellular medium. We report here the results of NMR measurements of the diffusion behavior of proteins expressed within bacterial cells, and find that these experiments provide a rapid and nondestructive probe of localization within cells and can be used to determine the size of the confining compartment. We show that diffusion can also be exploited as an editing method to eliminate extracellular species from high-resolution multidimensional spectra, and should be applicable to a wide range of problems. This approach is demonstrated here for a number of protein systems, using both (15)N and (13)C (methyl-TROSY) based acquisition.     

A detection-theoretic framework for modeling informational masking

There has been growing interest in recent years in masking that appears to have its origin at a central level of the auditory nervous system-so-called informational masking (IM). Masker uncertainty and target-masker similarity have been identified as the two major factors affecting IM; however, no theoretical framework currently exists that would give precise meaning to these terms necessary to evaluate their relative importance or model their effects. The present paper offers a first attempt at such a framework constructed within the doctrines of the theory of signal detection.     

Multi-residue method for the determination of chlorinated phenol metabolites in urine

Electron-capture-gas chromatographic (EC-GC) methods for the determination of chlorinated phenol metabolites of hexachlorobenzene (HCB) and pentachlorophenol (PCP) in urine are presented. After extraction the sample was reacted with diazomethane to produce the methyl ether of each metabolite prior to determination by EC-GC. An acid alumina column was used for cleanup and separation of methylated phenols into groups. Average recoveries of greater than 80% were obtained from urine fortified with known amounts of the phenol metabolites under investigation. A level of 1 ppb¹ was established as minimum detection limit for each phenol metabolite. Previously unreported urinary metabolites of HCB and PCP were found as a result of a rat feeding study. Levels of chlorinated phenol residues from (a) human general population and (b) a worker occupationally exposed to PCP are also included.     

Room-temperature phosphorescence,sensitized phosphorescence and fluorescence of licit and illicit drugs enhanced by organized media

The ability of microscopically organized media, in the form of surfactant micelles and α- and β-cyclodextrins, to enhance the luminescence phenomena of several licit and illicit drugs is discussed. Because physiological samples are not often amenable to direct spectrometric measurements without pretreatment, the applicability of these organized media to liquid chromatography is also considered. Fluorescence enhancements for certain hallucinogenic drugs such as N,N-dimethyltryptamine, mescaline and ibogaine are seen in cyclodextrin media compared to conventional, homogeneous solutions. Heavy-atom substituted sodium dodecyl sulfate micelles induce phosphorescence from cationic and/or hydrophobic drugs at room temperature in fluid solution; drugs such as propranolol, diflunisal, naphalozine, and selected quinoline derivatives can be determined conveniently. Sensitized phosphorescence is observed for several drugs including brethine, cocaine, didrate, estradiol, meprobarbital, methaqualone, phenobarbital, and sulfanilamide; it can be enhanced markedly when micellar solutions are used as the solvent. The energy-transfer step is facilitated by the organizing ability of the micelle; limits of detection can be decreased by over two orders of magnitude compared to homogeneous solvents. Sensitized phosphorescence can also be measured in cyclodextrin solutions, but the detectability is inferior to that in micellar media. Which form of organized medium is superior for determination of drugs is discussed.