PMID- 37968816 OWN - NLM STAT- MEDLINE DCOM- 20231127 LR - 20231127 IS - 1872-2059 (Electronic) IS - 1000-8713 (Print) IS - 1000-8713 (Linking) VI - 41 IP - 11 DP - 2023 Nov TI - [Determination of amanita peptide and tryptamine toxins in wild mushrooms by high performance liquid chromatography-tandem mass spectrometry]. PG - 976-985 LID - 10.3724/SP.J.1123.2023.07013 [doi] AB - The discovery and identification of mushroom toxins has long been an important area in the fields of toxicology and food safety. Mushrooms are widely favored for their culinary and medicinal value; however, the presence of potentially lethal toxins in some species poses a substantial challenge in ensuring their safe consumption. Therefore, the development of a robust and sensitive analytical method is necessary for accurately identifying the risks associated with mushroom consumption. The study of mushroom toxins, which are characterized by their diversity and substantial variations in chemical structures, present a considerable challenge for achieving precise and high-throughput analysis. To address this issue, the present study employed a robust approach combining a solid-phase extraction (SPE) purification technique with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) to establish an analytical method for the detection and quantification of five amatoxins and two tryptamines (psilocybin and bufotenine) present in some mushrooms. Several optimization procedures were undertaken, including optimizing the chromatographic conditions, mass spectrometric parameters, and sample extraction and purification. The procedure involved the extraction of dry mushroom powder with methanol containing 0.3% formic acid, followed by purification using a strong cation exchange cartridge (SCX). The analytes were separated on a T3 chromatographic column (100 mmx2.1 mm, 1.8 mum) using mobile phases of acetonitrile and 5 mmol/L ammonium acetate solution containing 0.1% formic acid. The multiple reaction monitoring (MRM) mode was employed for data acquisition. Amatoxins were quantified using matrix-matched standard calibration curves, whereas isotopic internal standards were used to quantify tryptamine. The results showed that all seven toxins exhibited good linearities (r(2)>0.99) within the optimized concentration range. The limits of detection (LODs) for bufotenine, psilocybin, and amatoxins were determined as 2.0, 5.0, and 10 mug/kg, respectively, while the limits of quantification (LOQs) were determined as 5.0, 10, and 20 mug/kg, respectively. The LOD and LOQ values further underscore the ability of the method to detect minute quantities of toxins, making it particularly well suited for screening food samples for potential contamination. Using dried shiitake mushroom powder as the matrix, the recoveries of the two tryptamines ranged from 80.6% to 117%, with relative standard deviations (RSDs) ranging from 1.73% to 5.98%, while the recoveries of amatoxins ranged from 71.8% to 115%, with RSDs varying from 2.14% to 9.92% at the three concentration levels. The consistent and satisfactory recoveries of amatoxins and tryptamines demonstrated the ability of this method to accurately quantify the target analytes even in a complex matrix. Comparison with the results of supplementary test method recognized by State Administration for Market Regulation for food (BJS 202008) demonstrated comparable results, indicating no significant differences (p>0.05) in amatoxin contents. The newly developed method is rapid, accurate, precise, meets the required standards, and is suitable for the detection of seven toxins in wild mushrooms. As part of the application of this method, a comprehensive investigation of the distribution of toxins in wild mushrooms from Fujian Province was undertaken. In this study, 59 wild mushroom samples from nine cities were collected in the Fujian province. Species identification was conducted using rDNA-internal transcribed space (rDNA-ITS) molecular barcode technology, which revealed the presence of toxins in the two samples. Notably, one specimen named Amanita fuligineoides contained alpha-amanitin, beta-amanitin, and phalloidin in quantities of 607, 377, and 69.0 mg/kg, respectively. Additionally, another sample, identified as Tricholomataceae, had a psilocybin concentration of 12.6 mg/kg. FAU - Liu, Lei-Qi AU - Liu LQ AD - School of Public Health, Fujian Medical University, Fuzhou 350122, China. AD - Fujian Provincial Key Laboratory for Zoonosis Research, Fujian Center for Disease Control and Prevention, Fuzhou 350012, China. FAU - Chen, Jing-Ze AU - Chen JZ AD - School of Public Health, Fujian Medical University, Fuzhou 350122, China. AD - Fujian Provincial Key Laboratory for Zoonosis Research, Fujian Center for Disease Control and Prevention, Fuzhou 350012, China. FAU - Fu, Wu-Sheng AU - Fu WS AD - School of Public Health, Fujian Medical University, Fuzhou 350122, China. AD - Fujian Provincial Key Laboratory for Zoonosis Research, Fujian Center for Disease Control and Prevention, Fuzhou 350012, China. AD - School of Pharmacy, Fujian University of Traditional Chinese Medicine, Fuzhou 350122, China. AD - Food Science College of Fujian Agriculture and Forestry University, Fuzhou 350002, China. FAU - Tang, Cui-Ying AU - Tang CY AD - Fujian Provincial Key Laboratory for Zoonosis Research, Fujian Center for Disease Control and Prevention, Fuzhou 350012, China. AD - School of Pharmacy, Fujian University of Traditional Chinese Medicine, Fuzhou 350122, China. LA - chi PT - English Abstract PT - Journal Article PL - China TA - Se Pu JT - Se pu = Chinese journal of chromatography JID - 9424804 RN - 0YIW783RG1 (formic acid) RN - 422ZU9N5TV (tryptamine) RN - 2RV7212BP0 (Psilocybin) RN - 0A31347TZK (Bufotenin) RN - 0 (Powders) RN - 0 (Mycotoxins) RN - 0 (Tryptamines) RN - 0 (DNA, Ribosomal) SB - IM MH - Chromatography, High Pressure Liquid MH - *Amanita/chemistry MH - Tandem Mass Spectrometry MH - Psilocybin MH - Bufotenin MH - Powders MH - *Mycotoxins MH - Tryptamines MH - DNA, Ribosomal PMC - PMC10654875 OTO - NOTNLM OT - amanitins OT - bufotenine OT - high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) OT - mushroom OT - phallotoxins OT - psilocin EDAT- 2023/11/16 06:44 MHDA- 2023/11/27 12:42 PMCR- 2023/11/08 CRDT- 2023/11/16 00:29 PHST- 2023/11/27 12:42 [medline] PHST- 2023/11/16 06:44 [pubmed] PHST- 2023/11/16 00:29 [entrez] PHST- 2023/11/08 00:00 [pmc-release] AID - 10.3724/SP.J.1123.2023.07013 [doi] PST - ppublish SO - Se Pu. 2023 Nov;41(11):976-985. doi: 10.3724/SP.J.1123.2023.07013.