Recent advances in all aspects of chromatography and separation science
These items appeared in the Liquid Chromatography section of Chromatography Abstracts.
2298 Subpicogram determination of (+)-anti-benzo[alpha]pyrene diol-epoxide adducts in fish albumin and globin by high-performance liquid chromatography with fluorescence detection.
Padros, J., Pelletier, E., Anal. Chim. Acta, 1 Jan 2001, 426(1), 71-77
A simple and highly sensitive HPLC/fluorescence method was developed for the determination of benzo[alpha]pyrene (BaP)-tetrol I-1 released after acid hydrolysis of (+)-anti-BaP diol-epoxide (BPDE)-blood protein adducts. This method does not require extensive tetrol isolation such as solvent extraction, multiple SPE columns and/or immunoaffinity chromatography. Instead, a single cleanup step using an inexpensive, disposable C18 SPE cartridge is performed, which yields 97% recovery of BaP-etrol-I-1. The method included a number of quality assurance measures and was validated using fish albumin (Alb) and globin (Gb) samples fortified with BaP-tetrol I-1. The absolute detection limit (S/N = 3) was 0.3 pg (0.9 fmol) per injection, corresponding to 450 fg (1.5 fmol)/mg Alb and 90 fg (0.3 fmol)/mg Gb for 1 ml of blood. The operating linear range was at least 1-100 pg (r2 = 0.99). Coefficients of variation for within-run and between-run assays were <5.5 and <9.3%, respectively. The method was applied to the determination of (+)-anti--BPDE-Alb and Gb adducts in fish intraperitoneally injected with a single (10 mg/kg) or two doses (25 mg/kg each) of BaP.
2299 Capillary liquid chromatographic determination of neutral phenolic compounds in apple juices.
Blanco Gomis, D., Fraga Palomino, N., Mangas Alonso, J. J., Anal. Chim. Acta, 1 Jan 2001, 426(1), 111-117
Capillary liquid chromatography (CLC) is evaluated as an alternative to conventional HPLC to analyse complex phenolics. Several neutral phenolic compounds were separated on a packed-reversed phase fused-silica capillary column, and determined with UV detection. Conventional liquid chromatographic equipment was adapted for such purposes. Application of the proposed method to the quantification of neutral phenols in apple juices is reported. Phenolics are extracted and fractionated into neutral and acidic compounds by means of a C18 solid-phase cartridge. Typical recoveries ranging from 90 to 105% are obtained and reproducibility between extractions is <7% in all cases. Mass detection limits are at the sub-nanogram level.