title: A rapid gas chromatographic injection-port derivatization method for the tandem mass spectrometric determination of patulin and 5-hydroxymethylfurfural in fruit juices.
abstract: A novel method consisting of injection-port derivatization coupled to gas chromatography-tandem mass spectrometry is described. The method allows the rapid assessment of 5-hydroxymethylfurfural (HMF) and patulin content in apple and pear derivatives. The chromatographic separation of the compounds was achieved in a short chromatographic run (12.2min) suitable for routine controls of these compounds in the fruit juice industry. The optimal conditions for the injection-port derivatization were at 270°C, 0.5min purge-off, and a 1:2 sample:derivatization reagent ratio (v/v). These conditions represent an important saving in terms of derivatization reagent consumption and sample preparation time. Quality parameters were assessed for the target compounds, giving LOD of 0.7 and 1.6μg/kg and LOQ of 2 and 5μg/kg for patulin and HMF, respectively. These values are below the maximum patulin concentration in food products intended for infants and young children. Repeatability (%RSD n=5) was below 12% for both compounds. In addition, the method linearity ranged between 25 and 1000μg/kg and between 5 and 192μg/kg for HMF and patulin, respectively. Finally, the method was applied to study HMF and patulin content in various fruit juice samples.
authors.affiliation: Departament de Química, Universitat de Lleida-Agrotecnio Center, Avda. Alcalde Rovira Roure, 191, E-25198, Lleida, Spain.
authors.forename: Alexis
authors.initials: A
authors.lastname: Marsol-Vall
authors.affiliation: Departament de Química, Universitat de Lleida-Agrotecnio Center, Avda. Alcalde Rovira Roure, 191, E-25198, Lleida, Spain.
authors.forename: Mercè
authors.initials: M
authors.lastname: Balcells
authors.affiliation: Departament de Química, Universitat de Lleida-Agrotecnio Center, Avda. Alcalde Rovira Roure, 191, E-25198, Lleida, Spain.
authors.forename: Jordi
authors.initials: J
authors.lastname: Eras
authors.affiliation: Departament de Química, Universitat de Lleida-Agrotecnio Center, Avda. Alcalde Rovira Roure, 191, E-25198, Lleida, Spain. Electronic address: canela@quimica.udl.cat.
authors.forename: Ramon
authors.initials: R
authors.lastname: Canela-Garayoa
mesh_terms: D000067030:Fruit and Vegetable Juices / Q000032:analysis*; D005662:Furaldehyde / Q000031:analogs & derivatives* / Q000032:analysis; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D027845:Malus / Q000737:chemistry; D010365:Patulin / Q000032:analysis*; D031989:Pyrus / Q000737:chemistry; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: C008046:5-hydroxymethylfurfural; D010365:Patulin; D005662:Furaldehyde
keywords: Fruit juices; GC–MS/MS; HMF; Injection-port derivatization; Patulin