Modified-QuEChERS-LC/MS method for the analysis of aflatoxins and ochratoxin A in coriander seeds.

Coriander seeds consumption, like other spices, has increased due to its culinary use, medicinal benefits, and its essential oil. However, there are few reports in the scientific literature on the prevalence of mycotoxins in this spice. In this report, an easy and simple method was proposed for the determination of the aflatoxin group (AFB1, AFB2, AFG1, and AFG2) and ochratoxin A (OTA) in coriander seeds. The recoveries of analytes ranged from 72 to 102% in spiked samples (0.5-5 µg/kg), with RSD below 11%. The limits of quantification (LOQ) are between 0.12 and 0.5 µg/kg. The proposed method represents an improvement compared to previous studies. It was tested for the determination of 13 samples, proving that it is fast, efficient, and sensitive. Only OTA was identified in four samples, all at levels lower than the European limits defined for some spices (0.88 and 5.4 µg/kg). Such methods are needed for monitoring these toxins in this spice to ensure consumer safety and provide insight into their occurrence.

A simple extraction method with no lipid removal for the determination of aflatoxins in almonds by liquid chromatography tandem-mass spectrometry (LC-MS/MS).

The present study describes a simple and rapid method for the determination of aflatoxins in almonds using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Aflatoxins were extracted using a modified QuEChERS method with little sample preparation, excluding the use of laborious purification procedures. Extracts were frozen overnight to separate the majority of lipids. The method was successfully validated for almonds. Linearity was demonstrated in the range 0.125-20 µg/kg. Limits of quantification (LOQ) ranged from 0.34 to 0.5 µg/kg. Matrix effect was not significant for the aflatoxins. Satisfactory recoveries were obtained at spike levels below 1 µg/kg and between 1 and 10 µg/kg. Relative standard deviations (RSDs) of repeatability and reproducibility were below 15%. The method was successfully tested with two proficiency tests in almond powder and peanut paste, with acceptable z-scores (-2 ≤ z ≤ 2). Only one of 11 local almond samples contained detectable aflatoxins, at concentrations below the maximum permitted level.

Chemometric Approach Based on Accuracy Profile and Data Chronological Distribution as a Tool to Detect Performance Degradation and Improve the Analytical Quality Control for Aflatoxins' Analysis in Almonds Using UPLC-MS/MS.

One of the main objectives of routine laboratories is the development of simple and reliable methods as well as meeting fit-for-purpose criteria for regulatory surveillance. In this study, the accuracy profiles and the evaluation of the distribution of results in the case of aflatoxins in almonds have been performed using ultraperformance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The method consists of designing the experiment and using certified reference material (CRM) to evaluate the bias, to calculate the combined uncertainty, and to construct the control charts. Good sensitivity (limit of quantifications (LOQs) 0.34-0.5 µg/kg) and recovery (between 82 and 107%) were achieved. The proposed method was successfully tested with a proficiency test in almond powder with acceptable z scores (-2 ≤ z ≤ 2). The results provided direct evidence for the proper functioning and stability of the whole analytical protocol, allowing acceptable combined uncertainty.

A facile extraction method followed by UPLC-MS/MS for the analysis of aflatoxins and ochratoxin A in raw coffee beans.

A UPLC-MS/MS method was developed and validated for the determination of aflatoxin B1 (AFB1), aflatoxin B2 (AFB2), aflatoxin G1 (AFG1), aflatoxin G2 (AFG2) and ochratoxin A (OTA) in raw coffee samples. Mycotoxins were extracted using a modified QuEChERS method with little sample preparation excluding clean-up and enrichment procedures. Linearity was demonstrated for the five mycotoxins in the range 0.125-20 µg/kg. This method shows negligible matrix effect for individual concentrations, thus allowing the use of an external standard procedure. Limits of quantification (LOQ) ranged from 0.45 to 1 µg/kg. Recoveries between 63% and 89% were achieved. The intra- and inter-day precisions were lower than 15%. The applicability of the method was demonstrated, taking into account fitness for purpose, with simplicity, reliability, low costs and environmental friendliness. The results show that 3 out of 4 samples were contaminated with OTA.