HPLC determination of pyroglutamic acid as a degradation product in parenteral amino acid formulations

Summary The aminoacid glutamine in aqueous solution and in conditions of high temperature and long term storage is partly transformed into pyroglutamic acid which exhibits potential neurotoxic effects.Commercially available aminoacid mixtures supplemented with glutamine are heat-sterilized and some losses of glutamine and formation of pyroglutamic acid may occur.The aim of the work was to set up an easy and reliable HPLC method which allows the determination of pyroglutamic acid as a degradation product of glutamine. The column was a 5 m Hypersil ODS (100×4.6 mm) and the mobile phase 100% 0.007 M phosphate buffer pH 3.5.Stability studies in different conditions of temperature and time of storage were performed on aminoacid mixture available in the commerce.     

Simultaneous microbatch screening of enantiorecognition on solid chiral selectors using selected mixtures of test-racemates: a case study on cellulose tris(alpha-phenylpropionate) with configurational diversity

An improved methodology for microbatch screening in the liquid-solid enantioselective adsorption of racemates by solid chiral selector is presented and illustrated by the evaluation of a series of six cellulose tris(alpha-phenylpropionate) presenting a configurational diversity and cellulose tris (4-methylbenzoate). Analyses were performed on 5 mg scale of chiral selector and 150 microL of supernatant containing a mixture of three test-racemates. Fifteen test-racemates were chosen according to their molecular diversity using a hierarchical clustering approach for seven selected three-dimensional molecular properties. The 15 racemates were sorted in five test mixtures composed of three racemates each according to the following constraints: each triplet of test-racemates can be analyzed without peak overlap on a commercially available chiral stationary phase (CSP). The designed five groups of three racemates may be used for the evaluation of other chiral selectors in view of the preparation of CSPs. This methodology improves the throughput of the evaluation and could be automated.     

Formation of ferrocyanides-IV Th(IV), Nd(III), UO(2)(II) and Hg(II)

The stoichiometry of the reaction between ferrocyanide and thorium, neodymium, uranyl ion and mercury(II) has been investigated. The first three give single products irrespective of the order of addition of the reagents, but the last does not. If mercury(II) is added to ferrocyanide Hg(2)Fe(CN)(6) is obtained, but if ferrocyanide is added to mercury(II) various cyanide complexes of mercury are formed. The K(sp) values for the precipitates are reported.     

Heterocyclic N-glycosyl derivatives—XIII: Reaction of 6-chloropurine and benzotriazoles with acetylated glycals

Acid-catalysed reactions of tri-O-acetyl-D-glucal with benzotriazole, 5,6-dimethylbenzotriazole, 5,6-dichlorobenzotriazole and 6-chloropurine have been found to give anomeric mixtures of the corresponding 2′,3′-unsaturated N-glycosyl derivatives with the α-anomers preponderating. When tri-O-acetyl-D-galactal was used the 3′,4′,6′-tri-O-acetyl-α- and β-D-lyxo-hexopyranosyl nucleoside analogs were obtained. The conformation and anomeric configuration of all the N-glycosyl compounds obtained were assigned by NMR studies.     

Consequence of boar edible tissue consumption on urinary profiles of nandrolone metabolites. II. Identification and quantification of 19-norsteroids responsible for 19-norandrosterone and 19-noretiocholanolone excretion in human urine

In previous work (Le Bizec et al., Rapid Commun. Mass Spectrom. 2000; 14: 1058), it was demonstrated that a boar meal intake could lead to possible false accusations of abuse of 17beta-nortestosterone in antidoping control. The aim of the present study was to identify and quantify endogenous 19-norsteroids in boar edible tissue at concentrations that can alter the steroid urinary profile in humans, and lead to excretion of 19-norandrosterone (19-NA) and 19-noretiocholanolone (19-NE). The samples were analysed in two laboratories. The methodologies used for extraction and detection (GC/MS(EI) and LC/MS/MS(APCI+)) are compared and discussed. 19-Norandrostenedione (NAED), 17beta- and 17alpha-nortestosterone (bNT, aNT), and 17beta- and 17alpha-testosterone (bT, aT) were quantified. The largest concentrations of NAED and bNT were observed in testicles (83 and 172 microg/kg), liver (17 and 63 microg/kg) and kidney (45 and 38 microg/kg). A correlation between the bNT and NAED content of a typical meal prepared with boar parts and the excreted concentrations of 19-NA and 19-NE in human urine was demonstrated.