MS/MS method for determining chloramphenicol residues in fish, shrimp, poultry, eggs, bovine and swine was developed and validated. The samples were extracted with a phosphate extraction solution followed by liquid-liquid extraction with ethyl acetate. The LC was performed on a C18 column at room te
A method for the determination of acrylamide in bakery products using ion trap LC-ESI-MS/MS
β Scribed by Achim Claus; Georg M. Weisz; Dietmar R. Kammerer; Reinhold Carle; Andreas Schieber
- Publisher
- John Wiley and Sons
- Year
- 2005
- Tongue
- English
- Weight
- 182 KB
- Volume
- 49
- Category
- Article
- ISSN
- 1613-4125
No coin nor oath required. For personal study only.
β¦ Synopsis
Acrylamide levels of bakery products, e. g., bread and bread rolls, are usually below 100 microg/kg , often even below 50 microg/kg. Therefore, usual analytical methods which have an LOQ greater, not dbl equals 25 microg/kg are not sensitive enough for detailed investigations on acrylamide formation within these commodities. An improved method for trace level determination of acrylamide in bakery products was developed using ion trap LC-ESI-MS/MS. Samples were divided into crumbs and crusts to achieve an initial concentration by removing the crumbs since these are devoid of acrylamide. After sample extraction and clean-up using multimode SPE cartridges, further analyte enrichment was accomplished by solid-phase-supported liquid-liquid extraction with ethyl acetate prior to LC-MS/MS analysis. The method was evaluated using bread, bread rolls, alkali-baked bread rolls, and toast. LOQ was calculated from the confidence interval of the calibration curve and found to be 1.7 ng/mL, corresponding to 17 microg/kg of product. When crumbs and crusts were separated, an LOQ of 10.2 microg/kg of bakery product could be obtained. As demonstrated in preliminary comparative analyses, accuracy of the method met the requirements for determination of trace level acrylamide formation in bakery products. Mean recovery was 102.4% (CV 4.5%), intermediate reproducibility revealed a CV of 2.1%, and a repeatability of CV 6.0%.
π SIMILAR VOLUMES
## Abstract A liquid chromatographyβelectrospray ionization tandem mass spectrometry (HPLCβESIβMS/MS) method for the quantitation of triamcinolone in human plasma after nasal spray application was developed and validated. Betamethasone was used as internal standard (IS). The analytes were extracted