Multi-mycotoxin Analysis of Finished Grain and Nut Products Using High-Performance Liquid Chromatography–Triple-Quadrupole Mass Spectrometry

Abstract

Mycotoxins in foods have long been recognized as potential health hazards due to their toxic and carcinogenic properties. A simple and rapid method was developed to detect 26 mycotoxins (aflatoxins, ochratoxins, fumonisins, trichothecenes, and ergot alkaloids) in corn, rice, wheat, almond, peanut, and pistachio products using high-performance liquid chromatography-triple-quadrupole mass spectrometry. Test portions of homogenized grain or nut products were extracted with acetonitrile/water (85:15, v/v), followed by high-speed centrifugation and dilution with water. Mean recoveries (± standard deviations) were 84 ± 6, 89 ± 6, 97 ± 9, 87 ± 12, 104 ± 16, and 92 ± 18% from corn, rice, wheat, almond, peanut, and pistachio products, respectively, and the matrix-dependent instrument quantitation limits ranged from 0.2 to 12.8 μg/kg, depending on the mycotoxin. Matrix effects, as measured by the slope ratios of matrix-matched and solvent-only calibration curves, revealed primarily suppression and were more pronounced in nuts than in grains. The measured mycotoxin concentrations in 11 corn and wheat reference materials were not different from the certified concentrations. Nineteen mycotoxins were identified and measured in 35 of 70 commercial grain and nut products, ranging from 0.3 ± 0.1 μg/kg (aflatoxin B1 in peanuts) to 1143 ± 87 μg/kg (fumonisin B1 in corn flour). This rapid and efficient method was shown to be rugged and effective for the multiresidue analysis of mycotoxins in finished grain and nut products.

Multi-mycotoxin Analysis of Finished Grain and Nut Products Using Ultrahigh-Performance Liquid Chromatography and Positive Electrospray Ionization–Quadrupole Orbital Ion Trap High-Resolution Mass Spectrometry

“…The "dilute-and-shoot" procedure used for the UHPLC/Q-orbital trap MS multianalysis of mycotoxins had been previously applied to and validated using HPLC-MS/MS. 17 To determine the optimal resolution setting, native mycotoxins were fortified in solvent (acetonitrile/water) and extracts obtained from acetonitrile/water extracts of mycotoxin-free peanut and wheat samples at 1, 10, and 100 ng/mL. Replicate measurements (n = 9) of these solutions were performed by operating the UHPLC/Q-orbital trap MS in full-scan mode and using R FWHM settings of 17 500, 35,000, 70 000, and 140 000.…”

“…Electrospray ionization in positive mode was used to ionize the mycotoxins and is the determining factor for detection since the orbital trap MS results were comparable to previous HPLC-MS/MS results using the same mycotoxins, matrices, and method. 17 Regulatory limits of deoxynivalenol and fumonisins determined by most countries and the European Union are in the 500−1000 μg/kg range, whereas aflatoxins and ochratoxin A limits are set at 20 and 50 μg/kg, respectively, in most grains and nut products. 28 As shown in Table 3, the method can achieve MD-ILQs a factor of at least 50 times lower than the MRLs required by the published regulatory requirements, which can be applied for screening purposes.…”

“…The performance and practical applicability of UHPLC/Q-orbital trap MS will be assessed by evaluating a validated procedure used to analyze, quantitate, and identify 26 mycotoxins in commercially available finished grain and nut products and reference grain materials by LC-MS/MS. 17 This hybrid technology has already been applied to screening mycotoxins in dairy products in full-scan mode. 18 Finished samples will be screened using full-scan MS, and identification of mycotoxins is achieved by data-dependent MS/MS experiment (DDMS 2 ) using the hybrid Q-orbital trap MS technology.…”

Multi-mycotoxin analysis of animal feed and animal-derived food using LC–MS/MS system with timed and highly selective reaction monitoring

“…For each analyte, the two most abundance product ions were simultaneously optimized on the mass spectrometer using a solvent-only standard [24,36]. However, some matrix co-extracts produced significant interference for the two selected product ions when complex samples were analyzed.…”

Study of the genetic diversity of the aflatoxin biosynthesis cluster inAspergillussectionFlaviusing insertion/deletion markers in peanut seeds from Georgia, USA

“…In the United States, Georgia is the main producer, with over 49% of the national total (http://nationalpeanutboard.org). Numerous agricultural products, including pistachio, almond, maize, fig, hazelnut, and peanut, have been reported to contain aflatoxins (Spanjer et al 2008;Liao et al 2013). These carcinogenic substances are secondary metabolites produced by multiple species from section Flavi, including Aspergillus flavus and A. parasiticus (Horn 2007).…”