National Food Institute, Technical University of Denmark, Denmark.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2009 Jul;26(7):1013-23. doi: 10.1080/02652030902806144.
A method for the simultaneous determination of 33 pesticides or degradation products together with patulin in apples by liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed. The method involved homogenization of the apples, extraction with ammonium acetate-acetic acid solution in methanol-water by ultrasonication, filtration, and determination by LC-MS/MS. The repeatability and within-laboratory reproducibility for the three spiking levels 0.02, 0.04 and 0.2 mg kg(-1) were between 4% and 35%. In general, the repeatability and reproducibility were about 10-20%. The limits of quantification (LOQs) were between 0.01 and 0.14 mg kg(-1). The method was used on incurred samples from parts of the ISAFRUIT project financed by the European Commission under the 6th Framework Programme. Samples were analysed at four different stages: after harvest, after storage (controlled), after a water bath, and after 28 days at room temperature. Pesticide residues were found at all stages, but no significant differences in the concentration were seen between the stages analysed. The concentration decreased significantly only for tolylfluanid after storage at room temperature for 28 days when only 0-6% of the original amount of tolylfluanid remained in the apples. No patulin was found in the apples stored for 28 days at room temperature and no growth of Penicillium expansum was observed on these apples. However, when the apples were inoculated with a spore suspension of P. expansum, high concentrations of patulin were found.
建立了一种同时测定苹果中 33 种农药或降解产物以及棒曲霉素的液相色谱-串联质谱（LC-MS/MS）方法。该方法包括苹果匀浆、甲醇-水混合液中的乙酸铵-乙酸超声提取、过滤和 LC-MS/MS 测定。三个加标水平（0.02、0.04 和 0.2 mg/kg）的重复性和实验室内再现性在 4%至 35%之间。一般来说，重复性和再现性约为 10-20%。定量限（LOQ）在 0.01 至 0.14 mg/kg 之间。该方法用于由欧盟第 6 框架计划资助的 ISAFRUIT 项目部分地区产生的样品。样品在四个不同阶段进行分析：收获后、储存（控制）后、水浴后和室温下储存 28 天后。在所有阶段都发现了农药残留，但分析的阶段之间没有浓度差异。仅在室温下储存 28 天后，甲苯氟磺胺的浓度显著下降，只有 0-6%的原始甲苯氟磺胺留在苹果中。在室温下储存 28 天的苹果中未发现棒曲霉素，也未观察到扩展青霉在这些苹果上生长。然而，当苹果被扩展青霉孢子悬浮液接种时，发现了高浓度的棒曲霉素。
