Analysis of oxytetracycline, tetracycline, and chlortetracycline in water using solid-phase extraction and liquid chromatography-tandem mass spectrometry

A method using liquid chromatography-tandem mass spectrometry has been developed for determination of trace levels of tetracycline antibiotics in ground water and confined animal feeding operation waste water. Oxytetracycline (OTC), tetracycline (TC), and chlortetracycline (CTC) were extracted from water samples using both polymeric and C18 extraction cartridges. The addition of a buffer containing potassium phosphate and citric acid improved tetracycline recoveries in lagoon water. Method detection limits determined in reagent water fortified with 1 microg l(-1) OTC, TC, and CTC were 0.21, 0.20, and 0.28 microg l(-1). Method detection limits in lagoon water samples fortified at 20 microg l(-1) for OTC, TC, and CTC were 3.6, 3.1, and 3.8 microg l(-1). Variability in recovery from laboratory fortified blanks ranged from 86 to 110% during routine analysis.     

Synthesis of substituted 2-amino-4-quinazolinones via ortho-fluorobenzoyl guanidines

A novel route to 12 substituted 2-amino-4-quinazolinones is described. Starting from 2,6-difluoro-4-methoxybenzonitrile, substitution of one of the fluorine atoms either directly or indirectly with heterocycles (e.g., pyridyl, thiazolyl, pyrazolyl) followed by hydrolysis of the nitrile gave a series of o-fluorobenzoic acid derivatives. Condensation with a set of six N,N-disubstituted guanidines followed by base-promoted ring closure afforded 2-amino-4-quinazolinone derivatives.     

Improvements in glass capillary gas chromatographic polychlorobiphenyl analysis

Separation of a 1:1:1:1 calibration mixture of Aroclors 1221, 1016, 1254, and 1260 on soda glass capillaries coated with Apolane (C-87) or Apiezon L is described. Polychlorobiphenyl congener structures are assigned to 112 separated and partially separated zones. The quantitative composition of Aroclor 1221 is reported. The performance of the two stationary phases on different lengths of laboratory and commercially prepared capillaries is compared and found to be very similar. Aroclors 1221, 1016, 1254, and 1260 are employed (1:1:1:1) for the primary calibration mixture because they contain all components of the commercial materials which pollute the environment; they are also easily obtained from the U.S. EPA Repository so that the method can be used in any laboratory by employing the calibration data given here.     

The Trp cage: folding kinetics and unfolded state topology via molecular dynamics simulations

Using over 75 mus of molecular dynamics simulation, we have generated several thousand folding simulations of the 20-residue Trp cage at experimental temperature and solvent viscosity. A total of 116 independent folding simulations reach RMSDcalpha values below 3 A RMSDcalpha, some as close as 1.4 A RMSDcalpha. We estimate a folding time of 5.5+/-3.5 mus, a rate that is in reasonable agreement with experimental kinetics. Finally, we characterize both the folded and unfolded ensemble under native conditions and note that the average topology of the unfolded ensemble is very similar to the topology of the native state.     

Measurement of the neutron lifetime using a proton trap

We report a new measurement of the neutron decay lifetime by the absolute counting of in-beam neutrons and their decay protons. Protons were confined in a quasi-Penning trap and counted with a silicon detector. The neutron beam fluence was measured by capture in a thin 6LiF foil detector with known absolute efficiency. The combination of these simultaneous measurements gives the neutron lifetime: tau(n)=(886.8+/-1.2[stat]+/-3.2[syst]) s. The systematic uncertainty is dominated by uncertainties in the mass of the 6LiF deposit and the 6Li(n,t) cross section. This is the most precise measurement of the neutron lifetime to date using an in-beam method.     

Precision neutron interferometric measurement of the nd coherent neutron scattering length and consequences for models of three-nucleon forces

We have performed the first high precision measurement of the coherent neutron scattering length of deuterium in a pure sample using neutron interferometry. We find b(nd)=(6.665+/-0.004) fm in agreement with the world average of previous measurements using different techniques, b(nd)=(6.6730+/-0.0045) fm. We compare the new world average for the nd coherent scattering length b(nd)=(6.669+/-0.003) fm to calculations of the doublet and quartet scattering lengths from several modern nucleon-nucleon potential models with three-nucleon force (3NF) additions and show that almost all theories are in serious disagreement with experiment. This comparison is a more stringent test of the models than past comparisons with the less precisely determined doublet scattering length of (2)a(nd)=(0.65+/-0.04) fm.     

Search for second-generation leptoquark pairs in &pmacr;p collisions at radicals = 1.8 TeV

We have searched for second-generation leptoquark (LQ) pairs in the &mgr;&mgr;+jets channel using 94+/-5 pb(-1) of &pmacr;p collider data collected by the D0 experiment at the Fermilab Tevatron during 1993-1996. No evidence for a signal is observed. These results are combined with those from the &mgr;nu+jets and nunu+jets channels to obtain 95% confidence level (C.L.) upper limits on the LQ pair production cross section as a function of mass and beta, the branching fraction of a LQ decay into a charged lepton and a quark. Lower limits of 200(180) GeV/c(2) for beta = 1(1 / 2) are set at the 95% C.L. on the mass of scalar LQ. Mass limits are also set on vector leptoquarks as a function of beta.     

Effect of ortho‐methylation on a bis(4‐cyanatocumyl)benezene low‐dielectric resin

A synthesis procedure for and characterization of a tetra‐ortho‐methyl substituted three‐ringed cyanate ester monomer, 4,4′‐[1,3‐phenylenebis(1‐methylethylidene)]bis[2,6‐dimethyl]phenylcyanato, and the corresponding cured resin are described with comparative characterization of the resin analogue without the ortho‐methyl substitutents. The othro‐methylation lowered the dielectric from 2.64 to 2.59 at 1 GHz and from 2.64 to 2.48 GHz at 15 GHz, whereas the tan δ was not significantly affected. Other physical properties also affected included a 40 °C decrease in the glass‐transition temperature, an increase in the thermal‐expansion coefficients, and a reduction in thermogravimetric stability. © 2002 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 41: 60–67, 2003     

Determination of total primary amines in seawater and plant nectar with flow injection sample processing and fluorescence detection

Flow injection sample processing is used with fluorescence detection for the determination of total primary amines in seawater and nectar. The effects of carrifer stream flow rate and dispersion tube length on sensitivity and sampling rates were studied. Relative responses of several amino acids and other primary amines were determined using two dispersion tube lengths. Linear calibration curves were obtained over the ranges 0–10^-6 M and O–1O^-5 M glycine. Precisions of better than 2% at 10^-6 M and a detection limit of 1 × lO^-8 M glycine were obtained. Applications to the analysis of seawater from the vicinity of a baited lobster trap and diluted nectar samples from Erythrina sp. are described.