PMID- 27442910 OWN - NLM STAT- MEDLINE DCOM- 20170321 LR - 20181224 IS - 1944-0057 (Electronic) IS - 1944-0057 (Linking) VI - 33 IP - 8 DP - 2016 Aug TI - High-performance liquid chromatography-tandem mass spectrometry method for simultaneous detection of ochratoxin A and relative metabolites in Aspergillus species and dried vine fruits. PG - 1355-66 LID - 10.1080/19440049.2016.1209691 [doi] AB - A simple, sensitive and reliable quantification and identification method was developed for simultaneous analysis of ochratoxin A (OTA) and its related metabolites ochratoxin alpha (OTalpha), ochratoxin B (OTB) and mellein. The method was assessed by spiking analytes into blank culture media and dried vine fruits. Performance was tested in terms of accuracy, selectivity and repeatability. The method involves an ultrasonic extraction step for culture samples using methanol aqueous solution (7:3, v/v); the mycotoxin is quantified by high-performance liquid chromatography coupled with electrospray ionisation and triple quadrupole mass spectrometry (LC-ESI-MS/MS). The recoveries were 74.5-108.8%, with relative standard deviations (RSDs) of 0.4-8.4% for fungal culture. The limits of detection (LODs) were in the range of 0.03-0.87 mug l(-)(1), and the limits of quantification (LOQs) ranged from 0.07 to 2.90 mug l(-)(1). In addition, the extraction solutions and clean-up columns were optimised specifically for dried vine fruit samples to improve the performance of the method. Methanol-1% sodium bicarbonate extraction solution (6:4, v/v) was determined to be the most efficient. Solid-phase extraction (SPE) was performed as a clean-up step prior to HPLC-MS/MS analysis to reduce matrix effects. Recoveries ranged from 80.1% to 110.8%. RSDs ranged from 0.1% to 3.6%. LODs and LOQs ranged from 0.06 to 0.40 mug kg(-)(1) and from 0.19 to 1.20 mug kg(-)(1), respectively. The analytical method was established and used to identify and quantify OTA and related compounds from Aspergillus carbonarius and Aspergillus ochraceus in cultures and dried vine fruits. The results showed that A. carbonarius produced OTalpha, OTB and OTA, whereas A. ochraceus produced OTB, OTA and mellein after 7 days of cultivation. Of 30 commercial samples analysed, 10 were contaminated with ochratoxins; OTB, OTalpha and mellein were also detected in different samples. FAU - Zhang, Xiaoxu AU - Zhang X AD - a College of Food Science and Nutritional Engineering , China Agricultural University , Beijing , China. FAU - Li, Jingming AU - Li J AD - a College of Food Science and Nutritional Engineering , China Agricultural University , Beijing , China. FAU - Cheng, Zhan AU - Cheng Z AD - a College of Food Science and Nutritional Engineering , China Agricultural University , Beijing , China. FAU - Zhou, Ziying AU - Zhou Z AD - b Supervision, Inspection & Testing Center of Agricultural Products Quality , Ministry of Agriculture , Beijing , China. FAU - Ma, Liyan AU - Ma L AD - a College of Food Science and Nutritional Engineering , China Agricultural University , Beijing , China. AD - b Supervision, Inspection & Testing Center of Agricultural Products Quality , Ministry of Agriculture , Beijing , China. LA - eng PT - Journal Article DEP - 20160721 PL - England TA - Food Addit Contam Part A Chem Anal Control Expo Risk Assess JT - Food additives & contaminants. Part A, Chemistry, analysis, control, exposure & risk assessment JID - 101485040 RN - 0 (Ochratoxins) RN - 16281-39-3 (5-chloro-8-hydroxy-3,4-dihydro-3-methylisocoumarin-7-carboxylic acid) RN - 1779SX6LUY (ochratoxin A) RN - ECJ5WS94N2 (ochratoxin B) RN - Y30Y67M5SV (ochracin) SB - IM MH - Aspergillus/*chemistry/metabolism MH - Chromatography, High Pressure Liquid MH - Fruit/*chemistry/metabolism MH - Ochratoxins/*analysis/*metabolism MH - Tandem Mass Spectrometry MH - Vitis/*chemistry OTO - NOTNLM OT - Ochratoxin alpha OT - liquid chromatography-tandem mass spectrometry OT - mellein OT - ochratoxin B OT - simultaneous extraction EDAT- 2016/07/22 06:00 MHDA- 2017/03/23 06:00 CRDT- 2016/07/22 06:00 PHST- 2016/07/22 06:00 [entrez] PHST- 2016/07/22 06:00 [pubmed] PHST- 2017/03/23 06:00 [medline] AID - 10.1080/19440049.2016.1209691 [doi] PST - ppublish SO - Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2016 Aug;33(8):1355-66. doi: 10.1080/19440049.2016.1209691. Epub 2016 Jul 21.