Rapid confirmatory method for the determination of sixteen synthetic growth promoters and bisphenol A in bovine milk using dispersive solid-phase extraction and liquid chromatography-tandem mass spectrometry.
A rapid liquid chromatographic-tandem mass spectrometric (LC-MS/MS) multi-residue method for the simultaneous quantitation and identification of sixteen synthetic growth promoters and bisphenol A in bovine milk has been developed and validated. Sample preparation was straightforward, efficient and economically advantageous. Milk was extracted with acetonitrile followed by phase separation with NaCl. After centrifugation, the extract was purified by dispersive solid-phase extraction with C18 sorbent material. The compounds were analysed by reversed-phase LC-MS/MS using both positive and negative ionization and operated in multiple reaction monitoring (MRM) mode, acquiring two diagnostic product ions from each of the chosen precursor ions for unambiguous confirmation. Total chromatographic run time was less than 10 min for each sample. The method was validated at a level of 1 microg L(-1). A wide variety of deuterated internal standards were used to improve method performance. The accuracy and precision of the method were satisfactory for all analytes. The confirmative quantitative liquid chromatographic tandem mass spectrometric (LC-MS/MS) method was validated according to Commission Decision 2002/657/EC. The decision limit (CCalpha) and the detection capability (CCbeta) were found to be below the chosen validation level of 1 microg L(-1) for all compounds.
Malone
E M
EM
The State Laboratory, Young's Cross, Celbridge, Co. Kildare, Ireland. edward.malone@statelab.ie
Elliott
C T
CT
Kennedy
D G
DG
Regan
L
L
D000818:Animals; D001559:Benzhydryl Compounds; D002417:Cattle; D008892:Milk / Q000737:chemistry*; D010636:Phenols / Q000032:analysis*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D052616:Solid Phase Extraction / Q000379:methods*; D013256:Steroids / Q000032:analysis*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D000098826:Bisphenol A Compounds
D001559:Benzhydryl Compounds; D010636:Phenols; D013256:Steroids; C006780:bisphenol A; D000098826:Bisphenol A Compounds