This study reports a robust and sensitive method for rapid testing of patulin in apple and apple juice. The method involved extraction of homogenised samples (10 g) with ethyl acetate (10 mL) and clean up by dispersive-solid phase extraction using primary secondary amine (25 mg/mL). Prior to the LC-MS/MS analysis, the cleaned extract was reconstituted in methanol/water (2:8). The optimised LC-MS condition provided a symmetric peak of patulin within a short LC-runtime of 5 min. The recoveries at the limit of quantification (0.005 mg/kg) and higher levels were satisfactory (> 80%), with the precision-RSD_r (< 11%). In an inter-laboratory comparison study involving 13 accredited laboratories, the reproducibility-RSD_R and HorRat values ranged between 4.80 and 6.08% and between 0.18 and 0.23 respectively, indicating a satisfactory method-precision. The z-scores of the participating laboratories were within ± 2. When the method was applied to incurred samples, the contamination range was 0.008–0.225 mg/kg and 0.018–0.034 mg/kg for apple and juice respectively, demonstrating a satisfactory performance in terms of precision. Based on the solvent standard, matrix-matched standard and standard-addition approaches, the calibration graphs provided similar quantitative performances. Because of its reliability, robustness and time-effectiveness, the method can be recommended for regulatory testing purposes.

本研究报告了一种快速检测苹果和苹果汁中展青霉素的稳健而灵敏的方法。该方法包括用乙酸乙酯 (10 mL) 萃取均质样品 (10 g) 并使用伯仲胺 (25 mg/mL) 通过分散固相萃取进行净化。在进行 LC-MS/MS 分析之前，将清洁的提取物在甲醇/水 (2:8) 中复溶。优化的 LC-MS 条件在 5 分钟的短 LC 运行时间内提供了棒曲霉素的对称峰。定量限 (0.005 mg/kg) 和更高水平的回收率令人满意 (> 80%)，RSD _r精度(< 11%)。在一项涉及 13 个认可实验室的实验室间比较研究中，重现性-RSD _R和 HorRat 值分别介于 4.80 和 6.08% 之间以及 0.18 和 0.23 之间，表明方法精密度令人满意。参与实验室的 z 值在 ± 2 以内。当该方法应用于产生的样品时，苹果和果汁的污染范围分别为 0.008-0.225 mg/kg 和 0.018-0.034 mg/kg，表明在精度方面。基于溶剂标准、基质匹配标准和标准添加方法，校准图提供了类似的定量性能。由于其可靠性、稳健性和时效性，该方法可推荐用于监管测试目的。