ABSTRACT
A simple and rapid liquid chromatography tandem mass spectrometry (LC-ESI-MS-MS) confirmation method for the analysis chloramphenicol (CAP) in milk powder has been developed. Samples were extracted by using liquid-liquid extraction steps with ethyl acetate. Lipids were removed using hexsan. LC separation was achieved by using a Phenomenex Luna C-18 column and acetonitryle-water as a mobile phase. The mass spectrometer was operated in multiple reaction monitoring mode (MRM) with negative electro-spray interface (ESI-). The four transitions were monitored m/z 321-->257, 321-->194, 321-->152, 326-->157 (IS) and for quantification, the transition m/z 321-->152 was chosen. Validation of the method was done according to criteria of Decision Commission No 2002/657 EC. Validation includes the determination of specification, linearity, precision (within- and between-day), accuracy, decision limit (CC alpha) and detection capability (CC beta). Samples were fortified at CAP levels 0.30, 0.45 and 0.60 microg/kg with CAP-5d as internal standard. The precision within-day (RSD%) was lower than 12% and accuracy (RE%) ranged from -9.8 to -3.7%. The precision between-day (RSD%) was less than 15%. The limit of decision (CC alpha) and detection capability (CC beta) for milk powder 0.09 and 0.11 microg/kg. Value CC alpha and CC beta were calculated for the 321-->152 ion transition. This method has been successfully used for routine analysis.
Subject(s)
Chloramphenicol/analysis , Chromatography, Liquid/methods , Food Contamination/analysis , Milk/chemistry , Spectrometry, Mass, Electrospray Ionization/methods , Animals , Anti-Bacterial Agents/analysis , Powders , Time FactorsABSTRACT
A method for benzoic acid determination in soft drinks by liquid chromatography using UV detector is presented. The method makes the possibility of benzoic acid determination with recovery about 95% and with variability index about 2.6%.
Subject(s)
Benzoates/analysis , Carbonated Beverages/analysis , Food Preservatives/analysis , Benzoic Acid , Chromatography, High Pressure Liquid/methodsABSTRACT
Residues of organochlorine pesticides in fat of game bagged in Eastern Poland in years 1988-1989 were determined. They were found to be smaller than the analogous residues in years 1986-1987.
Subject(s)
Adipose Tissue, Brown/chemistry , Artiodactyla , Hydrocarbons, Chlorinated , Insecticides/chemistry , Pesticide Residues/chemistry , Animals , PolandABSTRACT
The results are presented of the determinations of the content of organic chlorine pesticides in the perirenal fat tissue in wild animals killed in the years 1986-1987. The obtained mean values were similar to those found in our country in the 1980s.
Subject(s)
Adipose Tissue/analysis , Animals, Wild , Hydrocarbons, Chlorinated/analysis , Pesticide Residues/analysis , Animals , PolandABSTRACT
The results are presented of determinations of organic chlorine pesticides (sigma DDT, sigma BHC, HCB) in the perirenal fat of slaughtered animals. The study was done in the years 1986-1987 in East Poland.
