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| Rapid Determination of Patulin in Apple Juices by a Graphitized Carbon Black-based SPE Cartridge Coupled with HPLC－PDA and LC－MS/MS |
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| DOI： |
| KeyWord:graphitized carbon black patulin apple juice cleanup HPLC－PDA LC－MS/MS |
| Author | Institution |
| ZHANG Qiao-yan，ZHANG Xiao-feng，LI Ke，WANG Xia-jun，SHUAI Da-yao，GU Yu-ting |
1. Institute of Agro-product Safety and Nutrition，Zhejiang Academy of Agricultural Sciences，Hangzhou ，China; 2. Zhejiang Academy of Science and Technology for Inspection and Quarantine， Hangzhou ，China; 3. Zhejiang Rid Anzheng Testing and Certification;Technology Co.，Ltd.，Hangzhou ，China |
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| Abstract: |
| By virtue of the strong adsorption on patulin，a graphitized carbon black-based solid phase extraction （SPE） cartridge（named as GCB cartridge） was fabricated in this paper．Meanwhile，the GCB cartridge was combined with high performance liquid chromatography－photodiode array detector（HPLC－PDA） and liquid chromatography－tandem mass spectrometry（LC－MS/MS） in turn to evaluate the cleanup effects of the home-made GCB cartridge and four commercial SPE cartridges（Retain AX，PAX，MAX and HLB），which were further applied to analysis on the various impurities in the clear apple juice that could affect the accurate quantification of patulin．The significantly improved chromatograms obtained，signal-to-noise ratios（S/Ns） and matrix effects displayed their capabilities in the decrease of impurity interference．Among them，the GCB cleanup provided an ideal chromatogram in HPLC－PDA analyses，as well as an acceptable matrix effect of -14%，a chromatogram superior to the HLB cleanup and a comparable S/N to the Retain AX cleanup in LC－MS/MS analyses．Consequently，a LC－MS/MS method with the stable isotope dilution assay（SIDA－LC－MS/MS） was developed to overcome the impacts of matrix effect and cleanup loss on the accuracy of test results．The performance characteristics of methods based on different SPE cleanups with HPLC－PDA and SIDA－LC－MS/MS，respectively，were compared．The results showed that the GCB cleanup provided a higher sensitivity than the HLB cleanup due to its lower limits of detection and quantitation，while the methods with MAX，HLB and GCB cleanup all showed better recoveries（82%－102%） and smaller relative standard deviations（≤ 9%）．The developed GCB cleanup only needed two steps（i.e. loading and elution） to carry out by gravity on a SPE manifold within 10 min，which is simpler and faster than other SPE cleanups．The powerful cleanup effects were also reflected in the pigment removal of eight familiar apple juices．Furthermore，some locally moldy apples were processed into the apple juice which was verified to be a positive sample of 34 μg·kg-1 patulin by the GCB cleanup and the analyses by HPLC－PDA and SIDA－LC－MS/MS，respectively．The better cleanup effects and lower cost of GCB cartridge would be helpful to its wide application in the routine detection of patulin. |
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