No abstract

A new method has been developed for estimation of recoverable oil in citrus juices, based on quantitative combination in acid solution of d-limonene, the principal component of distilled citrus oils, with bromine. 2-Propanol is added to citrus juice, the mixture is distilled, and the distillate is acidified with HC1 and titrated with potassium bromate-bromide solution. End point is observed by disappearance of color from methyl orange indicator. The distillation requires about 3 min., and complete determination, less than 7 min. Recovery of added d-limonene was 100 ±1%, indicating a high degree of accuracy; replications seldom varied more than 0.001% oil, indicating excellent precision. Recoveries were consistently higher than by the Clevenger method.

No abstract

A procedure to assess the bioavailability of persistent organic pollutants (POPs) from soil samples has been developed. The procedure is based on the use of simulated in vitro gastrointestinal extraction to remove POPs from soil matrices. The level of recovery, using this approach, is assessed following liquid-liquid extraction (LLE) and analysis by gas chromatography-mass selective detection (GC-MSD). The remaining soil residue is then extracted using pressurised fluid extraction (PFE) followed by GC-MSD analysis to assess the residual fraction. The residual fraction is monitored to determine the unavailable fraction i.e. not available for absorption in the gastrointestinal tract of humans. The procedure was applied to four soil samples i.e. an aged, spiked soil and three certified reference materials (CRMs) contaminated with POPs. Recoveries of pesticides (lindane, endosulfan I, endrin, DDE, DDD and endosulfan II), phenols (cresol, TCP and PCP), and base neutral compounds (hexachloroethane, acenaphthene, dibenzofuran, fluorene and hexachlorobenzene) from aged, spiked soil following extraction with gastric fluid ranged from 0.8 to 8.3% while following intestinal extraction ranged from 5.5 to 13.5%, irrespective of POP. Recoveries of pesticides (lindane, endosulfan I, endrin, DDE, DDD and endosulfan II) from CRM 805-050 following extraction with gastric fluid were below the limit of detection while following intestinal extraction ranged from 5.3 to 12.8%. Recoveries of phenols (cresol, TCP and PCP) from CRM 401-225 following extraction with gastric fluid ranged from 1.6 to 2.0% while following intestinal extraction ranged from 4.1 to 5.4%. Recoveries of base neutral acid analytes (hexachloroethane, acenaphthene, dibenzofuran, fluorene and hexachlorobenzene) from CRM 107-100 following extraction with gastric fluid ranged from 1.4 to 4.0% while following intestinal extraction ranged from 6.6 to 12.7%. It has been found that the majority of POPs present i.e. >75%, would be excreted if consumed and not be absorbed in the gastrointestinal tract of humans.

An attempt is made to determine the bioavailability of persistent organic pollutants (POP's) in environmental matrices. The approach is based on the use of the Hildebrand Solubility Parameter, and its individual parameters of hydrogen bonding, dispersion and polarity to select weak and strong solvents to extract POP's from soil matrices. The approach has been applied to both spiked soils and certified reference materials. Initial results indicate that it is possible to fractionate POP's from soil matrices based on their ability to be extracted from soil by particular solvents.