鲜食苹果中棒曲霉素HPLC检测及前处理条件的优化

Optimization on HPLC detection and pre-treatment conditions of patulin in fresh apple

为建立快速、准确的鲜食苹果中棒曲霉素含量检测方法,试验以红富士苹果为试材,分别研究不同HPLC条件对分离效果的影响,不同提取方法及纯化技术对鲜食苹果中棒曲霉素提取效果的影响。结果表明：在流动相配比为乙腈∶水=10∶90,流速0.8 mL/min的HPLC条件下,鲜食苹果样品中棒曲霉素色谱峰达到最好的分离效果;在不同的提取方法中,直接研磨提取法获得最高的加标回收率（81.9%）,PEP-SPE技术较普通液液萃取技术具有更高的加标回收率（82.42%~95.57%）及检测精密度（3.26%~4.41%）,同时具有更方便、快捷的特点。综上,研究建立的PEP-SPE—HPLC技术可操作性强,结果准确,具有很好的适用性,为鲜食苹果中棒曲霉素的含量检测及有效控制提供了灵敏高效的测定方法。

A rapid and sensitive method was established for the accurate determination of patulin in fresh apples.Experimental parameters including extraction methods,mobile phase composition and flow rate for HPLC which always affect the sensitivity and analysis efficiency of the method were optimized systemically.The results indicated that solid phase extraction（SPE）techniques using functionalized polystyrene-divinylbenzene column（PEP）exhibited satisfactory recoveries comparing with other extraction methods.Under the optimized chromatographic conditions,patulin could be well separated from other impurities within 4min,and detected with a wide linear range between 10-25 000μg/L and a detection limit of 10μg/L（S/N=3）using acetonitrile/water（90：10,v/v）as mobile phase,0.8mL/min as flow rate.The proposed PEP-SPE-HPLC method was further applied to the determination of patulin in fresh apples in the range of 82.42%-95.57%,indicating it might serve as an efficient tool for the accurate quantification of patulin in food samples.