Optimization and Validation of a Method Without Alkaline Clean-Up for Patulin Analysis on Apple Puree Agar Medium (APAM) and Apple Products

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• 作者：Nikki De Clercq ; Els Van Pamel ; Els Van Coillie…
• 关键词：Patulin ; Apple products ; Liquid ; liquid extraction (LLE) ; Solid ; phase extraction (SPE) clean ; up ; HPLC ; UV
• 刊名：Food Analytical Methods
• 出版年：2016
• 出版时间：February 2016
• 年：2016
• 卷：9
• 期：2
• 页码：370-377
• 全文大小：813 KB
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• 作者单位：Nikki De Clercq (1)
  Els Van Pamel (1)
  Els Van Coillie (1)
  Geertrui Vlaemynck (1)
  Frank Devlieghere (2)
  Bruno De Meulenaer (3)
  Els Daeseleire (1)
  
  1. Institute for Agricultural and Fisheries Research (ILVO), Member of Food2Know, Brusselsesteenweg 370, 9090, Melle, Belgium
  2. Faculty of Bioscience Engineering, Department of Food Safety and Food Quality, Laboratory of Food Microbiology and Food Preservation, Member of Food2Know, Ghent University, Coupure Links 653, 9000, Ghent, Belgium
  3. Faculty of Bioscience Engineering, Department of Food Safety and Food Quality, Laboratory of Food Chemistry and Human Nutrition, Member of Food2Know, Ghent University, Coupure Links 653, 9000, Ghent, Belgium
  
• 刊物类别：Chemistry and Materials Science
• 刊物主题：Chemistry
  Food Science
  Chemistry
  Microbiology
  Analytical Chemistry
  
• 出版者：Springer New York
• ISSN：1936-976X

文摘

A sensitive high-performance liquid chromatography-UV (HPLC-UV) method, based on the Association of Analytical Communities (AOAC) Official method 2000.02, was developed and validated for the high-throughput analysis of patulin in in vitro experiments on apple puree agar medium (APAM). The importance of repeating the ethyl acetate extraction step at liquid-liquid extraction (LLE) was examined, as well as the extent of patulin degradation during the sodium carbonate clean-up. In addition to this alkaline clean-up, the efficiency of using an Oasis HLB or C₁₈ cartridge as solid-phase extraction (SPE) clean-up was compared. This resulted in a two-step ethyl acetate LLE, followed by an Oasis HLB SPE clean-up, without alkaline clean-up conditions. The method was fully validated for APAM, cloudy apple juice, and apple puree. Average patulin recoveries at levels of 100, 500, and 1000 μg kg−1 of APAM varied between 95 and 113 % over 3 independent days, with an interday precision (RSD_R) of 5 to 10 %. Recovery experiments carried out with the spiked apple juice (at 50 μg kg−1) and apple puree (10 μg kg−1) showed average recovery rates laying between 80–101 % (RSD_R = 12 %) and 77–100 % (RSD_R = 9 %), respectively. This method offered a detection limit of 3–4 μg kg−1 and a quantification limit of 5–8 μg kg−1 for APAM, apple juice, and puree.