Determination of organochlorine compounds in fatty matrices. Application of rapid off-line normal-phase liquid chromatographic clean-up.
A clean-up method for organochlorine compounds in fatty samples based on normal-phase liquid chromatography (NPLC) is described. To this end, an existing clean-up procedure which uses column switching for the separation of organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs) from the fat matrix was simplified to a single silica LC column procedure. The use of an LC column packed with 3 microns silica enables complete fat/OCP separation in a total fraction volume of 12 ml, and results in a fully automated clean-up procedure that takes only 32 min per sample. The method showed average recoveries of 80-110% in the concentration range of 1-510 micrograms/kg, with relative standard deviations of less than 10%. Limits of determination were in the range of 0.5-50 micrograms/kg. The simplified approach has shown its potential for a variety of samples, such as milk, pork fat, animal feed and cod liver oil, showing its general applicability to fatty samples.
van der Hoff
G R
GR
National Institute of Public Health and Environmental Protection (RIVM), Bilthoven, Netherlands.
van Beuzekom
A C
AC
Brinkman
U A
UA
Baumann
R A
RA
van Zoonen
P
P
D000273:Adipose Tissue / Q000737:chemistry; D000821:Animal Feed / Q000032:analysis; D000818:Animals; D002849:Chromatography, Gas / Q000379:methods*; D002853:Chromatography, Liquid / Q000379:methods*; D003060:Cod Liver Oil / Q000032:analysis; D004041:Dietary Fats / Q000032:analysis*; D006801:Humans; D006843:Hydrocarbons, Chlorinated / Q000032:analysis* / Q000302:isolation & purification; D007306:Insecticides / Q000032:analysis* / Q000302:isolation & purification; D008895:Milk, Human / Q000737:chemistry; D011078:Polychlorinated Biphenyls / Q000032:analysis* / Q000302:isolation & purification; D015203:Reproducibility of Results; D013056:Spectrophotometry, Ultraviolet; D013552:Swine
D004041:Dietary Fats; D006843:Hydrocarbons, Chlorinated; D007306:Insecticides; D003060:Cod Liver Oil; D011078:Polychlorinated Biphenyls