Determination of chlormequat in pig serum and sow milk by LC-MS/MS.
Chlormequat is a plant growth regulator widely used on cereals, and there is general concern that it may impair human fertility. A LC-MS/MS method for the analysis of chlormequat in milk and serum was developed and validated in connection with an investigation on the effect of chlormequat on pig reproduction. Validation of the method was based on recovery tests at three spiking levels, determined as double determinations and repeated at least four times. Samples were extracted with methanol-water-acetic acid, centrifuged, filtrated and determined by LC-MS/MS. The mean recoveries were in the range 80-110%, and the LOD was 0.2 ng/g for serum and 0.3 ng/g for milk. The values for repeatability and reproducibility were within 2/3 of the limits given by the Horwitz equation. Samples of pig serum (59) and sow milk (27) were analyzed using the method. Chlormequat was determined in four milk samples in the range of 0.4 ng/g to 1.2 ng/g and in all serum samples in the range of 0.2 ng/g-4.0 ng/g.
Poulsen
M E
ME
National Food Institute, Danish Technical University, Mørkhøj Bygade 19, 2860 Søborg, Denmark. mep@food.dtu.dk
Christensen
H B
HB
Sørensen
M T
MT
Leffers
H
H
Andersen
J H
JH
D000818:Animals; D002716:Chlormequat / Q000032:analysis*; D002853:Chromatography, Liquid / Q000379:methods; D005504:Food Analysis; D005506:Food Contamination / Q000032:analysis*; D013058:Mass Spectrometry / Q000379:methods; D008892:Milk / Q000737:chemistry*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013552:Swine / Q000097:blood*
D002716:Chlormequat