Alternaria is a genus of fungi which grows on fruit and vegetables, responsible for producing a series of low molecular weight metabolites, named Alternaria toxins. In 2011 EFSA expressed its scientific opinion on the risk for animals and public health associated with the presence of these toxins[1]. Later the Recommendation (EU) 2022/553 established the indicative levels for some Alternaria toxins in various food products as tomatoes[2]. In this context, an analytical method based on liquid chromatography coupled to tandem mass spectrometry was validated for the determination of five toxins in sundried tomatoes: Alternariol (AOH), Alternariol Monomethyl Ether (AME), Tenuazoic acid (TeA), Tentoxin (TEN) and Altenuene (ALT). These toxins were extracted from the sample with a solution of methanol/water/acetic acid and subsequently an aliquot of the extract was purified on a Strata-XL column. After the elution with methanol, the Alternaria toxins were analyzed using a 6500+ QTRAP triple quadrupole spectrometer equipped with an Ion Drive source in negative ion mode. The chromatographic separation was performed with a Kinetex EVO C18 column using 5 mM ammonium acetate buffer and methanol as mobile phases in a gradient program. The validation was performed according to the performance criteria mentioned by Regulation (EU) 2017/625 and the following parameters were considered: specificity, limit of detection and quantification (LOD and LOQ), linearity, repeatability, reproducibility, accuracy, and uncertainty.[3] LOD and LOQ were respectively in the range of 0.1-0.23 and 0.1-1.3 µg/kg, satisfying the requirements established by European legislation. The recovery rates were between 73% and 104% with a relative standard deviation of intra-laboratory reproducibility below 13%. References: 1. EFSA on Contaminants in the Food Chain (CONTAM). EFSA Journal, 9 (2011) 2407. 2. Commission Recommendation (EU) 2022/553 of 5 April 2022 on monitoring the presence of Alternaria toxins in food. Off. J. Eur. Union L 107:90. 3. Regulation (EU) 2017/625 of the European Parliament and of the Council of 15 March 2017 on official controls and other official activities performed to ensure the application of food and feed law, rules on animal health and welfare, plant health and plant protection products. Off. J. Eur. Union L 95:1
VALIDATION OF METHOD FOR THE DETERMINATION OF ALTERNARIA TOXINS IN SUNDRIED TOMATOES BY LC-MS/MS
Loredana Annunziata;Rosaria Aloia;C. Chaves Lopez;
2023-01-01
Abstract
Alternaria is a genus of fungi which grows on fruit and vegetables, responsible for producing a series of low molecular weight metabolites, named Alternaria toxins. In 2011 EFSA expressed its scientific opinion on the risk for animals and public health associated with the presence of these toxins[1]. Later the Recommendation (EU) 2022/553 established the indicative levels for some Alternaria toxins in various food products as tomatoes[2]. In this context, an analytical method based on liquid chromatography coupled to tandem mass spectrometry was validated for the determination of five toxins in sundried tomatoes: Alternariol (AOH), Alternariol Monomethyl Ether (AME), Tenuazoic acid (TeA), Tentoxin (TEN) and Altenuene (ALT). These toxins were extracted from the sample with a solution of methanol/water/acetic acid and subsequently an aliquot of the extract was purified on a Strata-XL column. After the elution with methanol, the Alternaria toxins were analyzed using a 6500+ QTRAP triple quadrupole spectrometer equipped with an Ion Drive source in negative ion mode. The chromatographic separation was performed with a Kinetex EVO C18 column using 5 mM ammonium acetate buffer and methanol as mobile phases in a gradient program. The validation was performed according to the performance criteria mentioned by Regulation (EU) 2017/625 and the following parameters were considered: specificity, limit of detection and quantification (LOD and LOQ), linearity, repeatability, reproducibility, accuracy, and uncertainty.[3] LOD and LOQ were respectively in the range of 0.1-0.23 and 0.1-1.3 µg/kg, satisfying the requirements established by European legislation. The recovery rates were between 73% and 104% with a relative standard deviation of intra-laboratory reproducibility below 13%. References: 1. EFSA on Contaminants in the Food Chain (CONTAM). EFSA Journal, 9 (2011) 2407. 2. Commission Recommendation (EU) 2022/553 of 5 April 2022 on monitoring the presence of Alternaria toxins in food. Off. J. Eur. Union L 107:90. 3. Regulation (EU) 2017/625 of the European Parliament and of the Council of 15 March 2017 on official controls and other official activities performed to ensure the application of food and feed law, rules on animal health and welfare, plant health and plant protection products. Off. J. Eur. Union L 95:1I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.
