PMID- 24091376 OWN - NLM STAT- MEDLINE DCOM- 20140512 LR - 20131004 IS - 1873-4324 (Electronic) IS - 0003-2670 (Linking) VI - 799 DP - 2013 Oct 17 TI - Development of a sensitive and reliable high performance liquid chromatography method with fluorescence detection for high-throughput analysis of multi-class mycotoxins in Coix seed. PG - 68-76 LID - S0003-2670(13)01139-2 [pii] LID - 10.1016/j.aca.2013.08.042 [doi] AB - As an edible and medicinal plant, Coix seed is readily contaminated by more than one group of mycotoxins resulting in potential risk to human health. A reliable and sensitive method has been developed to determine seven mycotoxins (aflatoxins B1, B2, G1, G2, zearalenone, alpha-zearalenol, and beta-zearalenol) simultaneously in 10 batches of Coix seed marketed in China. The method is based on a rapid ultrasound-assisted solid-liquid extraction (USLE) using methanol/water (80/20) followed by immunoaffinity column (IAC) clean-up, on-line photochemical derivatization (PCD), and high performance liquid chromatography coupled with fluorescence detection (HPLC-FLD). Careful optimization of extraction, clean-up, separation and detection conditions was accomplished to increase sample throughput and to attain rapid separation and sensitive detection. Method validation was performed by analyzing samples spiked at three different concentrations for the seven mycotoxins. Recoveries were from 73.5% to 107.3%, with relative standard deviations (RSDs) lower than 7.7%. The intra- and inter-day precisions, expressed as RSDs, were lower than 4% for all studied analytes. Limits of detection and quantification ranged from 0.01 to 50.2 mug kg(-1), and from 0.04 to 125.5 mug kg(-1), respectively, which were below the tolerance levels for mycotoxins set by the European Union. Samples that tested positive were further analyzed by HPLC tandem electrospray ionization mass spectrometry for confirmatory purposes. This is the first application of USLE-IAC-HPLC-PCD-FLD for detecting the occurrence of multi-class mycotoxins in Coix seed. CI - Copyright (c) 2013 Elsevier B.V. All rights reserved. FAU - Kong, Wei-Jun AU - Kong WJ AD - Key Laboratory of Bioactive Substances and Resources Utilization of Chinese Herbal Medicine, Ministry of Education, Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences & Peking Union Medical College, Beijing 100193, China. FAU - Li, Jun-Yuan AU - Li JY FAU - Qiu, Feng AU - Qiu F FAU - Wei, Jian-He AU - Wei JH FAU - Xiao, Xiao-He AU - Xiao XH FAU - Zheng, Yuguo AU - Zheng Y FAU - Yang, Mei-Hua AU - Yang MH LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20130906 PL - Netherlands TA - Anal Chim Acta JT - Analytica chimica acta JID - 0370534 RN - 0 (Fluorescent Dyes) RN - 0 (Mycotoxins) SB - IM MH - Chromatography, High Pressure Liquid/*standards MH - Coix/*chemistry MH - Fluorescent Dyes/*chemistry MH - High-Throughput Screening Assays/*methods MH - Limit of Detection MH - Molecular Structure MH - Mycotoxins/*analysis MH - Reproducibility of Results MH - Seeds/*chemistry MH - Time Factors OTO - NOTNLM OT - Coix seed OT - High performance liquid chromatography-fluorescence detection OT - High-throughput analysis OT - Method development OT - Multi-class mycotoxin EDAT- 2013/10/05 06:00 MHDA- 2014/05/13 06:00 CRDT- 2013/10/05 06:00 PHST- 2013/06/26 00:00 [received] PHST- 2013/08/15 00:00 [revised] PHST- 2013/08/27 00:00 [accepted] PHST- 2013/10/05 06:00 [entrez] PHST- 2013/10/05 06:00 [pubmed] PHST- 2014/05/13 06:00 [medline] AID - S0003-2670(13)01139-2 [pii] AID - 10.1016/j.aca.2013.08.042 [doi] PST - ppublish SO - Anal Chim Acta. 2013 Oct 17;799:68-76. doi: 10.1016/j.aca.2013.08.042. Epub 2013 Sep 6.