Automated high-performance liquid chromatographic determination of chloramphenicol in milk and swine muscle tissue using on-line immunoaffinity sample clean-up.

An on-line high-performance liquid immunoaffinity chromatographic (HPLIAC) system for the direct determination of chloramphenicol in milk and swine muscle tissue is described. The system consisted of a dual-column system in which an HPLIAC column was directly coupled to an RP-8 high-performance liquid chromatographic column. Skimmed and deproteinated milk or aqueous muscle tissue extract was directly injected into the HPLIAC column. After a washing step with phosphate-buffered saline, chloramphenicol was desorbed by a glycine-NaCl buffer (pH 2.8) and directly concentrated on the RP-8 column. Next, chromatography was carried out using acetonitrile-sodium acetate buffer as the mobile phase. Chloramphenicol was detected at 280 nm. Mean recoveries from spiked raw milk were 70 +/- 2% (1-50 micrograms/kg) and from spiked swine muscle tissue 64 +/- 2% (10-50 micrograms/kg). The calibration curves were linear in the range 1-200 micrograms/kg spiking levels. Limits of determination were 1 microgram/kg for milk and 10 micrograms/kg for muscle tissue.     

Standardized methods for measuring radionuclides in drinking water

Summary In 2002 the Italian Standardisation Organisation (UNI) - Nuclear Energy Commission (UNICEN) - appointed a working group with the main task of writing a set of standards on drinking water measurements. To date two standards have been designed, namely, for total alpha- and beta-activity, and ²²²Rn. Further procedures are under development for measuring ²²⁶Ra and U isotopes, and gamma-emitting radionuclides in water. The paper gives an overview of these standards, both developed and under study, with special attention to the validation of the methods.     

Matter induced neutrino decay and solar antineutrinos

The properties of matter-induced neutrino decay with majoron emission are analysed in some details for the cases of Majorana, ZKM and Dirac neutrinos. The result of such a decay of solarv _e 's in the sun interior could be the appearance of \(\bar \nu _e \) flux. Assuming that the neutrinos have only standard weak interactions, the solar \(\bar \nu _e \) flux can be at the border of detectability for the future large volume detectors like Borex or Super-Kamiokande. However, the \(\bar \nu _e \) signal can be considerably larger, provided the neutrinos have new non-standard interactions with matter.     

New FIR laser lines from CD3OD optically pumped by a CO2 waveguide laser

In this work we report new FIR laser lines from CD₃OD optically pumped by a CO₂ waveguide laser. The wide tunability of this laser (290 MHz) makes it possible to pump absorption lines with large frequency offset relative to the CO₂ laser line center, which are not possible by using conventional CO₂ lasers. As a consequence 19 new laser lines have been discovered, ranging from 38.0 m to 455.2 m in wavelength. For all lines, precise frequency offset measurements between the CO₂ line center and the center of the absorber CD₃OD line were performed using the transferred Lamb-dip technique. We also present direct Doppler-free offset measurements of infrared absorption, obtained within the FIR laser cavity itself, using optoacoustic detection.Work supported by FAPESP, CNPq, FAP-Brasil and CNR-Italy     

Fast neutrino decay and solar neutrino detectors

The neutrino decay solution of the solar neutrino problem is revisited in the context of majoron models. It is shown that for a definite range of parameters this scenario reconciles both the Homestake and the Kamiokande data. The prediction for Gallium detectors is also given. Attention is devoted to the analysis of the signal, which is the crucial prediction of this scenario. It is shown that the sensitivity of Borexino is sufficient to observe this signal and to distinguish it from the alternative signal provided by hybrid models of neutrino oscillation and magnetic moment transitions. Other sources of solar production are also reviewed (matter induced decay, MSW catalized decay or the decay of solar 17 keV neutrinos).     

Prediction of retention times in linear gradient temperature and pressure programmed analysis on capillary columns

The simultaneous temperature and inlet pressure programming (TPP) in gas chromatographic analysis decreases the retention time and the maximum value of temperature required for the elution of high boiling substances. Therefore, compounds sensitive to thermal degradation can be better analysed and column ageing is reduced. However, the empirical choice of proper analysis conditions requires many preliminary runs; this paper describes a procedure for the theoretical prediction of retention times in TPP using few preliminary runs carried out in isobaric and isothermal conditions. The used program permits the prediction of the retention times of the compounds analysed with any different TPP run carried out within the temperature and pressure ranges investigated with the preliminary runs. The influence of various analytical parameters on the accuracy of the prediction values was investigated. The proposed model also predicts the relative position in the chromatogram of closely eluting peaks and the possible coincidence of retention times or inversion of the elution order with changing temperature. It is also possible to foresee the analytical conditions, which offer a baseline separation of all of the peaks of the sample.     

The selectivity and polarity of carbon layer open tubular capillary columns modified with a polar liquid phase

The polarity of carbon layer open tubular (CLOT) columns coated with a layer of non-porous graphitized carbon black (Carbopack B) modified with an appropriate amount of polar polyglycol liquid phase has been evaluated and compared with that of standard polar (Supelcowax-10) and non-polar (SPB-1) bonded phase open tubular columns. The efficiency and selectivity were measured at various temperatures and the polarity of the columns was evaluated by use of McReynolds' constants and the difference in apparent carbon number, ΔC of linear alkanes and alcohols. The polarity of the CLOT column was found to depend on temperature, and changing the analytical conditions therefore enabled the separation of compounds of different polarity whose reciprocal position and resolution were affected by temperature. The application of calculation methods which enable programmed temperature retention times to be predicted from isothermal data was also found to be possible when the polarity of the CLOT column changes with temperature.     

Asymmetric Alkylations of a Sultam-Derived Glycine Equivalent: Practical preparation of enantiomerically pure α-amino acids

Alkylation of the chiral glycine derivative 2 with “activated” organohalides under ultrasound-assisted phasetransfer catalysis or with activated and nonactivated organohalides in anhydrous medium provides (mostly crystalline) alkylation products 3 . Acidic hydrolysis of the pure products 3 gives (aminoacyl)sultams 4 which by mild saponification furnish pure α-amino acids 5 in good overall yields from 2 , along with recovered auxiliary 1 (Scheme 1). Pure ω-protected α,ω-diamino acids and α-amino-ω-(hydroxyamino)acids 12–16 are readily accessible from (ω-haloacyl)sultams 3 via reaction with N-nucleophiles followed by acidic and basic hydrolyses (Scheme 2). A reliable determination of the enantiomeric purity of α-amino acids using HPLC analysis of their N-(3,5-dinitrobenzoyl)prolyl derivatives 17 is presented.     

Structures of simarinolide and guanepolide (x-ray analysis), new quassinoids from Simaba cf orinocensis

Simarinolide $\text{4a}$ and Guanepolide $\text{5a}$ are new quassinoids with a C₂₅ basic skeleton isolated from a member of the French Guyanan Simaroubaceae, Simaba cf orinocensis H.B.K. The structure $\text{4a}$ was established by spectral means and that of $\text{5a}$ by X-ray diffraction analysis. The previously known simarolide $\text{1}$ was also isolated.     

Evaluation and prediction of the shape of gas chromatographic peaks

The evaluation and prediction of the shape of asymmetric gas chromatographic peaks is important as the knowledge of the amount of tailing permits to foresee the resolution between closely eluting peaks and to select the best analytical conditions for an efficient and rapid separation. A model function was tested in order to approximate the true peak shape obtained on non-polar column by injecting different compounds. The trend of the parameters involved in the used equation has been investigated as a function of column temperature and inlet pressure. The reproduction of the symmetrical or asymmetrical shape of gas chromatographic peaks is satisfactory and the method also permits to predict the shape of peaks obtained in different conditions of temperature and pressure.