Journal
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
Volume 407, Issue 18, Pages 5433-5442Publisher
SPRINGER HEIDELBERG
DOI: 10.1007/s00216-015-8705-3
Keywords
Patulin; Apple products; Multimode column; LC/MS; Isotope dilution mass spectrometry
Funding
- Korea Research Institute of Standards and Science [15011030]
Ask authors/readers for more resources
Patulin, a mycotoxin produced by several molds in fruits, has been frequently detected in apple products. Therefore, regulatory bodies have established recommended maximum permitted patulin concentrations for each type of apple product. Although several analytical methods have been adopted to determine patulin in food, quality control of patulin analysis is not easy, as reliable certified reference materials (CRMs) are not available. In this study, as a part of a project for developing CRMs for patulin analysis, we developed isotope dilution liquid chromatography-tandem mass spectrometry (ID-LC/MS/MS) as a higher-order reference method for the accurate value-assignment of CRMs. C-13(7)-patulin was used as internal standard. Samples were extracted with ethyl acetate to improve recovery. For further sample cleanup with solid-phase extraction (SPE), the HLB SPE cartridge was chosen after comparing with several other types of SPE cartridges. High-performance liquid chromatography was performed on a multimode column for proper retention and separation of highly polar and water-soluble patulin from sample interferences. Sample extracts were analyzed by LC/MS/MS with electrospray ionization in negative ion mode with selected reaction monitoring of patulin and C-13(7)-patulin at m/z 153 -> m/z 109 and m/z 160 -> m/z 115, respectively. The validity of the method was tested by measuring gravimetrically fortified samples of various apple products. In addition, the repeatability and the reproducibility of the method were tested to evaluate the performance of the method. The method was shown to provide accurate measurements in the 3-40 mu g/kg range with a relative expanded uncertainty of around 1 %.
Authors
I am an author on this paper
Click your name to claim this paper and add it to your profile.
Reviews
Recommended
No Data Available