title: Development and validation of ultra-high-performance liquid chromatography-tandem mass spectrometry methods for the simultaneous determination of beauvericin, enniatins (A, A1, B, B1) and cereulide in maize, wheat, pasta and rice.
abstract: Rapid and accurate UPLC-MS/MS methods for the simultaneous determination of beauvericin and the related enniatins (A, A1, B, B1), together with cereulide were successfully developed and validated in cereal and cereal-based food matrices such as wheat, maize, rice and pasta. Although these emerging foodborne toxins are of different microbial origin, the similar structural, toxicological and food safety features provided rationale for their concurrent detection in relevant food matrices. A Waters Acquity UPLC system coupled to a Waters Quattro Premier XE™ Mass Spectrometer operating in ESI+ mode was employed. Sample pretreatment involved a fast and simple liquid extraction of the target toxins without any further clean-up step. For all toxins the sample preparation resulted in acceptable extraction recoveries with values of 85-105% for wheat, 87-106% for maize, 84-106% for rice and 85-105% for pasta. The efficient extraction protocol, together with a fast chromatographic separation of 7min allowed substantial saving costs and time showing its robustness and performance. The validation of the developed method was performed based on Commission Decision 2002/657/EC. The obtained limits of detection ranged from 0.1 to 1.0μgkg-1and the limits of quantification from 0.3 to 2.9μgkg-1for the targeted toxins in the selected matrices. The obtained sensitivities allow detection of relevant toxicological concentrations. All relative standard deviations for repeatability (intra-day) and intermediate precision (inter-day) were lower than 20%. Trueness, expressed as the apparent recovery varied from 80 to 107%. The highly sensitive and repeatable validated method was applied to 57 naturally contaminated samples allowing detection of sub-clinical doses of the toxins.
authors: Department of Bioanalysis, Laboratory of Food Analysis, Ghent University, Ottergemsesteenweg 460, Ghent, Belgium; Department of Food Safety and Food Quality, Laboratory of Food Microbiology and Food Preservation, Ghent University, Coupure Links 653, Ghent, Belgium. Electronic address: marliesdecleer@gmail.com.
authors: Marlies
authors: M
authors: Decleer
authors: Department of Food Safety and Food Quality, Laboratory of Food Microbiology and Food Preservation, Ghent University, Coupure Links 653, Ghent, Belgium.
authors: Andreja
authors: A
authors: Rajkovic
authors: Department of Food Safety and Food Quality, Food2Know, Ghent University, Coupure Links 653, Ghent, Belgium.
authors: Benedikt
authors: B
authors: Sas
authors: Department of Organic Chemistry, Organic and Biomimetic Chemistry Research Group, Ghent University, Krijgslaan 281, Ghent, Belgium.
authors: Annemieke
authors: A
authors: Madder
authors: Department of Bioanalysis, Laboratory of Food Analysis, Ghent University, Ottergemsesteenweg 460, Ghent, Belgium.
authors: Sarah
authors: S
authors: De Saeger
mesh_terms: D002851:Chromatography, High Pressure Liquid; D047630:Depsipeptides / Q000032:analysis*; D002523:Edible Grain / Q000737:chemistry*; D005433:Flour; D005506:Food Contamination / Q000032:analysis*; D057230:Limit of Detection; D012275:Oryza / Q000737:chemistry; D006109:Poaceae / Q000737:chemistry*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014118:Toxins, Biological / Q000032:analysis; D014908:Triticum / Q000737:chemistry; D003313:Zea mays / Q000737:chemistry
chemical_list: D047630:Depsipeptides; D014118:Toxins, Biological; C089294:cereulide; C100264:enniatins; C004456:beauvericin
keywords: Cereulide; Cyclic depsipeptides; Emerging mycotoxins; Fusarium; LC–MS analysis; Solvent extraction