Development of bovine muscle, liver and urine reference materials for zeranol – preparation, homogeneity and stability

 Samples of bovine muscle, liver and urine, zeranol-free (RM 508, RM 509 and RM 510, respectively) and zeranol-containing (RM 511, RM 512 and RM 513, respectively) were prepared and tested as candidate reference materials. Preliminary studies on achievement of target zeranol content, intercomparison of analytical methods (HPLC-RIA and GC-MS) and effects of lyophilisation and irradiation on zeranol content are described. The preparation of the materials and testing for homogeneity and stability of zeranol in the materials are discussed. The coefficients of variation for zeranol determinations for between-vial homogeneity (4.0%, 4.4% and 4.6% for muscle, liver and urine, respectively) are similar to those for the analytical method (4.0%, 7.3% and 6.8% for muscle, liver and urine, respectively) indicating that the materials are homogeneous. Stability data over a 12-month storage period at temperatures ranging from −18 °C to +37 °C indicate that the materials are sufficiently stable for use as reference materials. This paper is dedicated to the memory of Dr Hilary Stevenson (The Queen’s University of Belfast/DANI) who, together with Mr. W. Graham, facilitated the irradiation of the lyophilised materials.--> Received: 18 June 1996/Revised: 19 August 1996/Accepted: 23 August 1996     

Highly regio- and stereo-specific preparation of a new carbohydrate-based 1,3-oxazin-2-one by the INIR method and its applications in some asymmetric transformations

Preliminary experiments show that a new gulonic acid-derived 1,3-oxazin-2-one, prepared by an intramolecular nitrene insertion reaction (INIR) method, serves to control both asymmetric aldol and Diels-Alder reactions with excellent stereo-selection.     

Anionic responses of electrochemically synthesized polypyrrole films

Conducting polypyrrole films with thickness of about 8 mum were prepared on platinum by continuous scanning in 0.1M pyrrole and 0.1M electrolyte (LiCl, LiBF(4) or NaBF(4)). Scan-rates of 10, 20 and 50 mV/sec with scan-times of 30, 45 and 60 min were used. The potentiometric response of the films was tested over a range of anions. Films were found to be anion-sensitive but very non-selective. The influence of the doping cation was also investigated.