A systematic assessment of the variability of matrix effects in LC-MS/MS analysis of ergot alkaloids in cereals and evaluation of method robustness
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- 作者：Svetlana V. Malysheva (1)
José Diana Di Mavungu (1)
Irina Yu Goryacheva (2)
Sarah De Saeger (1) - 关键词：Ergot alkaloids ; Matrix effect ; Robustness ; LC ; MS/MS
- 刊名：Analytical and Bioanalytical Chemistry
- 出版年：2013
- 出版时间：June 2013
- 年：2013
- 卷：405
- 期：16
- 页码：5595-5604
- 全文大小：846KB
- 参考文献：1. Komarova EL, Tolkachev ON (2001) The chemistry of peptide ergot alkaloids. Part 1. Classification and chemistry of ergot peptides. Pharm Chem J 35:37-5
2. Fuller GJ (1968) The day of St. Anthony's Fire. Signet
3. Krishnamachari KAVR, Bhat RV (1976) Poisoning by ergoty bajra (pearl millet) in man. Indian J Med Res 64:1624-628
4. Urga K, Debella A, Medihn YW, Agata N, Bayu A, Zewdie W (2002) Laboratory studies on the outbreak of gangrenous ergotism associated with consumption of contaminated barley in Arsi, Ethiopia. Ethiopian J Health Dev 16:317-23
5. Baumann U, Hinziker HR, Zimmerli B (1985) Ergot alkaloids in Swiss cereal products. Mitt Geb Lebensmittelunters Hyg 76:609-30
6. Dusemund B, Altmann HJ, Lampen A (2006) Mutterkornalkaloide in Lebensmitteln: II. Toxikologische Bewertung: Mutterkornalkaloid-kontaminierter Roggenmehle. Journal Verbraucherschutz Lebensmittel 1:150-52 CrossRef
7. Krska R, Crews C (2008) Significance, chemistry and determination of ergot alkaloids: a review. Food Addit Contam: Part A 25:722-31 CrossRef
8. Scott PM (2009) Ergot alkaloids: extent of human and animal exposure. World Mycotoxin J 2:141-49 CrossRef
9. Kokkonen M (2011) The challenge of LC/MS/MS multi-mycotoxin analysis—Heracles battling the Hydra? Academic dissertation. Presented, with the permission of the Faculty of Agriculture and Forestry, University of Helsinki, for public criticism in lecture hall B2, Viikki, on October 14th 2011. ISBN 978-952-225-096-4
10. Mohamed R, Gremauda E, Richoz-Payot J, Tabet J-C, Guya PA (2006) Quantitative determination of five ergot alkaloids in rye flour by liquid chromatography–electrospray ionisation tandem mass spectrometry. J Chrom A 1114:62-2 CrossRef
11. Krska R, Stubbings G, Macarthur R, Crews C (2008) Simultaneous determination of six major ergot alkaloids and their epimers in cereals and foodstuffs by LC–MS–MS. Anal Bioanal Chem 391:563-76 CrossRef
12. Diana Di Mavungu J, Malysheva SV, Sanders M, Larionova D, Robbens J, Dubruel P, Van Peteghem C, De Saeger S (2012) Development and validation of a new LC-MS/MS method for the simultaneous determination of six major ergot alkaloids and their corresponding epimers. Application to some food and feed commodities. Food Chem 135:292-03 CrossRef
13. Matuszewski BK, Costancer ML, Chaver-Eng CM (2003) Strategies for assessment of matrix effect in quantitative bioanalytical methods based on HPLC-MS/MS. Anal Chem 75:3019-030 CrossRef
14. Lenain P, Diana Di Mavungu J, Dubruel P, Robbens J, De Saeger S (2012) Development of suspension polymerized molecularly imprinted beads with metergoline as template and application in a solid phase extraction procedure towards ergot alkaloids. Anal Chem 84:10411-0418 CrossRef
15. Kokkonen M, Jestoi M (2010) Determination of ergot alkaloids from grains with UPLC-MS/MS. J Sep Sci 33:2322-327 CrossRef
16. Lauber U, Schnaufer R, Gredziak M, Kiesswetter Y (2005) Analysis of rye grains and rye cereals for ergot alkaloids. Mycotoxin Res 21:258-62 CrossRef
17. Sulyok M, Krska R, Schuhmacher R (2007) A liquid chromatography/tandem mass spectrometric multi-mycotoxin method for the quantification of 87 analytes and its application to semi-quantitative screening of moldy food samples. Anal Bioanal Chem 389:1505-523 CrossRef
18. Royer D, Humpf H-U, Guy PA (2004) Quantitative analysis of / Fusarium mycotoxins in maize using accelerated solvent extraction before liquid chromatography/atmospheric pressure chemical ionization tandem mass spectrometry. Food Addit Contam 21:678-92 CrossRef
19. Pierri L, Pitman IH, Rae ID, Winkler DA, Andrews PR (1982) Conformational analysis of the ergot alkaloids ergotamine and ergotaminine. J Med Chem 25:937-42 CrossRef
20. Smith DJ, Schappell NW (2002) Technical note: epimerization of ergopeptine alkaloids in organic and aqueous solvents. J Anim Sci 80:1616-622
21. Hafner M, Sulyok M, Schuhmacher R, Crews C, Krska R (2008) Stability and epimerisation behaviour of ergot alkaloids in various solvents. World Mycotoxin J 1:67-8 CrossRef - 作者单位：Svetlana V. Malysheva (1)
José Diana Di Mavungu (1)
Irina Yu Goryacheva (2)
Sarah De Saeger (1)
1. Laboratory of Food Analysis, Faculty of Pharmaceutical Sciences, Ghent University, Harelbekestraat 72, 9000, Ghent, Belgium
2. Department of General and Inorganic Chemistry, Chemistry Institute, Saratov State University, Astrakhanskaya 83, 410012, Saratov, Russia - ISSN：1618-2650
文摘
The study presents for the first time a systematic investigation of matrix effects in the LC-MS/MS analysis of ergot alkaloids in cereals. In order to assure the accuracy of the results, several approaches to minimize/eliminate matrix effects were investigated including variation of ionization techniques, chromatography and sample preparation on different grain types and grain varieties. It was revealed that the use of UPLC and careful choice of sample preparation might reduce signal suppression/enhancement. In general, ergometrine was found to be the most susceptible among the ergot alkaloids studied, but none of the used approaches suggested a total elimination of matrix effects; only less than half of its MS signal could be recovered. The late-eluting compounds were less affected by matrix components in all conditions tested. Further, the robustness of the applied LC-MS method was checked by means of a fractional factorial design. The results indicate that small changes to the sample preparation parameters, namely pH and concentration of extraction buffer, shaking time, drying temperature and extraction volumes, did not significantly (α--.05) affect the recoveries of ergot alkaloids. Figure SSE (%) applying different sample preparation procedures