Determination of 15 Mycotoxins in Foods and Feeds Using High Performance Liquid Chromatography-Tandem Mass Spectrometry with Gel Permeation Chromatography Combined QuEChERS Purification

Abstract

A reliable, sensitive and selective method was successfully developed to determine 15 different mycotoxins simultaneously in foods and feeds. In this method, the homogenized sample was first treated with gel permeation chromatography (GPC) to eliminate most of coextracts, such as pigments, lipids and waxes. A quick, easy, cheap, effective, rugged, and safe (QuEChERS) method was then carried out as a further cleaned up step, during which the polar interfering compounds such as organic acids and sugars were removed by vortexing with ODS in acetonitrile phase. Using double sample injection method, the analytes were separated by ZORBAX Eclipse plus C18 (1.8 µm, 2.1×100 mm) and detected by a MS/MS system with electrospray ionization (ESI) at multi-reaction monitoring (MRM) mode. The result indicated that the LOD of 15 mycotoxins were ranged from 0.07~5.0 µg/kg. Meanwhile, high correlation coefficients (r 2 >0.996) of 15 mycotoxins were obtained within their respective linear ranges. The average recoveries for lower, intermediate, and high spiked levels ranged from 80.1%~95.5% in company with RSD ranged from 10.5%~19.6%. The method not only represents many advantages including simple pre-treatment, good purification and high sensitivity, but also successfully fit the minimum limiting level requests from various countries including EU, USA and Japan.

Developments in mycotoxin analysis: an update for 2011-2012

“…An LC-MS/MS method to quantify aflatoxins, OTA and ZEA in cereals has been reported by Liao et al (2011), whereas Takino et al (2011) proposed an LC-MS/MS method for the simultaneous determination of DON, ZEA, T-2 and HT-2 in wheat and biscuits. The combination of gel permeation chromatography to eliminate co-extractants, such as pigments, lipids and waxes and QuEChERS for the removal of polar interfering compounds, such as organic acids and sugars, prior to LC-MS/MS analysis has been described by Gong et al (2012) for the determination of 15 mycotoxins in foods and feeds. An LC-MS/MS method for the simultaneous determination of aflatoxins, OTA, ZEA, DON, fumonisins, T-2 and HT-2 in cereals has been reported by Soleimany et al (2012a,b).…”

Review of QuEChERS Methods for the Analysis of Mycotoxins in Food Samples

“…A method, whichh was found to be sensitive, reliable, and selective was developed for the determination of 15 mycotoxins in foods and feeds using HPLC-MS with gel permeation chromatography combined with QuEChERS purification [22]. For the sample preparation, 10 g of each homogenized sample was transferred into a 100 ml centrifuge tube followed by addition of 40 ml of 84% (v/v) acetonitrile/water mixture and the mixture was homogenized for 3 min with high-speed homogenizer.…”

A Comparative Study of Fungal and Some Aflatoxin Contents of Freshly Fried and Stored <i>Sallah</i> Meat from Danbatta Local Government Area of Kano State, Nigeria

“…The residue was re-dissolved using 8 mL of a mixture of ethylacetate/cyclohaxane (50:50 v/v), filtered with 0.45 μm nylon filter paper, the filtrate was again dried using a rotary evaporator and the residue was then re-dissolved in 1 mL of methanol/10 mMol/L ammonium acetate (1:1 v/v). Finally, the solution was passed through 0.22 μm nylon filter paper prior to injection into the HPLC [44]. The excitation and emission wavelengths for the aflatoxin detection were set at 360 nm and 450 nm, respectively.…”

“…The injection volume was 20 μl, and the gradient elution was used in Liquid Chromatographic step with a mobile phase consisting of solvent A (10 mmol/L ammonium acetate was used for the ESI+ mode and 0.1% (v/v) aqueous ammonia was used for the ESI-mode) and solvent B (methanol) at follow rates: 0 -2.0 min, 40% B -60% B; 2.0 -7.0 min 60% B -95% B; 7.0 -9.0 min, 95% B; 9.0 -9.5 min, 95% B -40% B. A subsequent re-equilibration time (2 min) was performed before the next injection [44].…”