Enrichment of benzo[a]pyrene in smoked food products and determination by high-performance liquid chromatography-fluorescence detection.

We developed a procedure for trace enrichment of benzo[a]pyrene (BP) in extracts of smoked food products, and an HPLC-fluorescence detection (FL) method for determination of BP in the enriched extracts. The procedure consists in extraction/sonication of the lyophilized product in hexane, clean-up of the hexane extract by passage through a Sep-Pak Silica Plus cartridge and, subsequently, by partitioning between hexane and dimethyl sulphoxide, and concentration of the BP using a Sep-Pak C18 Plus cartridge. HPLC-FL and quantification limits were 0.049 microgram/l in acetonitrile (< 0.0067 microgram/kg of smoked food) and 0.089 microgram/l in acetonitrile (< 0.012 microgram/kg), respectively. Recovery (94.1%) and RSD (< 8.65%) were satisfactory. When applied to 15 types of sausage, mean BP content was 0.022 microgram/kg, and all but two samples (both treated with wood smoke) had BP contents below the 0.03 microgram/kg limit imposed in EU legislation for smoking-flavour agents.

Determination of benzo[a]pyrene in lipid-soluble liquid smoke (LSLS) by HPLC-FL.

We developed a method for the determination of low levels of the carcinogen benzo[a]pyrene (BaP) in lipid-soluble liquid smoke (LSLS). The method consists of partitioning the LSLS (2 g) between n-hexane and DMSO, purification of the DMSO extracts on Sep-Pak C18 Plus and then Silica Plus cartridges, and determination of the BaP in the isolated extract by HPLC with fluorescence detection. Detection and quantification limits were 0.049 microgram/l (0.024 microgram/kg of LSLS) and 0.089 microgram/l (0.045 mg/kg), respectively. Recovery (87%) and CV% (< or = 1.5) were satisfactory.

Second-derivative constant-wavelength synchronous scan spectrofluorimetry for determination of benzo[b]fluoranthene, benzo[a]pyrene and indeno[1,2,3-cd]pyrene in drinking water.

The use of derivative constant-wavelength synchronous scan fluorimetry is reported for the determination of three polycyclic aromatic hydrocarbon pollutants in drinking water (linearity range 0.4-4 mug 1(-1)). The limits of detection (LD) and quantification (LQ) (mug 1(-1)) are 0.01 and 0.07 for benzo[b]fluoranthene, 0.03 and 0.12 for benzo[a]pyrene and 0.19 and 0.57 for indeno[1,2,3-cd]pyrene in the presence of three other pollutants, benzo[k]fluoranthene, benzo[ghi]perylene and fluoranthene. The precision (RSD /= 85%) were satisfactory.

Determination of Benzo[a]pyrene in smoking-flavour agents (water-soluble liquid smoke) by second derivative constant-wavelength synchronous spectrofluorimetry.

We have developed a simple, rapid, inexpensive method for the determination of benzo[a]pyrene (BP, a known carcinogen) in smoking-flavour agents (water-soluble liquid smoke; WSLS). After purification of the WSLS by a single passage through a Sep Pak C18 Plus cartridge, BP in the hexane eluate was determined by second derivative constant-wavelength synchronous spectrofluorimetry. Method precision (RSD < 6%) and recovery ( approximately 92%) were satisfactory, and the detection and quantification limits (1.05 and 2.28 mug kg(-1) respectively) indicated that the current maximum permissible concentration of BP in smoke flavourings (10 mug kg(-1)) can be monitored by this method.

Synchronous spectrofluorimetric determination of total amounts of the six polycyclic aromatic hydrocarbons officially designated as indicators of drinking water quality.

We report a quick, simple method for determination of the joint concentration of the 6 polycyclic aromatic hydrocarbons (PAHs) designated by current legislation as quality indicators for drinking water and for surface waters destined for use as drinking water. Water samples are extracted with hexane, and total indicator PAH concentration is determined by synchronous spectrofluorimetry (optimal instrumental parameters are reported). The detection limit (5.0 ng/L), quantitation limit (8.4 ng/L), precision (coefficient of variation, 3.8%), and accuracy (recovery, 77%) were well within the legal bounds for reference methods.