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A useful strategy based on chromatographic data combined with quality-by-design approach for food analysis applications. The case study of furanic derivatives in sugarcane honey
Journal of Chromatography A ( IF 4.1 ) Pub Date : 2017-09-08 , DOI: 10.1016/j.chroma.2017.09.019
Pedro Silva , Catarina L. Silva , Rosa Perestrelo , Fernando M. Nunes , José S. Câmara

Sugarcane honey (SCH) is one of the Madeira Island products par excellence and it is now popular worldwide. Its sui generis and peculiar sensory properties, explained by a variety of volatile compounds including furanic derivatives (FDs), arise mainly from manufacturing and storage conditions. A simple high-throughput approach based on semi-automatic microextraction by packed sorbent (MEPS) combined with ultra-high performance liquid chromatography (UHPLC) was developed and validated for identification and quantification of target FDs in sugarcane honey. A Quality-by-Design (QbD) approach was used as a powerful strategy to optimize analytical conditions for high throughput analysis of FDs in complex sugar-rich food matrices. The optimum point into MEPS-Method Operable Design: Region (MODR) was obtained with R-CX sorbent, acetonitrile (ACN) as elution solvent, three loading cycles and 500 μL of sample volume. The optimum point into UHPLC-MODR was obtained with a CORTECS column operating at a temperature of 50 °C, ACN as eluent and a flow rate of 125 μL min−1. The robustness was demonstrated by Monte Carlo simulation and capability analysis for estimation of residual errors. The concentration-response relationship for all FDs were described by polynomial function models, being confirmed by Fisher variance (F-test). The% recoveries were in a range of 91.9-112.1%. Good method precision was observed, yielding relative standard deviations (RSDs) less than 4.9% for repeatability and 8.8% for intermediate precision. The limits of quantitation for the analytes ranged from 30.6 to 737.7 μg kg−1. The MEPSR-CX/UHPLCCORTECS-PDA method revealed an effective and potential analytical tool for SCH authenticity control based on target analysis of FDs allowing a strict control and differentiation from other similar or adulterated products.



中文翻译:

一种基于色谱数据并结合按质量设计方法进行食品分析应用的有用策略。甘蔗蜂蜜中呋喃衍生物的研究

甘蔗蜂蜜(SCH)是马德拉岛卓越的产品之一,现已在全球范围内广受欢迎。它的特殊性包括呋喃衍生物(FDs)在内的多种挥发性化合物可以解释其特殊的感官特性,其主要源于制造和储存条件。建立了一种简单的高通量方法,该方法基于装填吸附剂(MEPS)与超高效液相色谱(UHPLC)结合的半自动微萃取,并已用于鉴定和定量甘蔗蜂蜜中的目标FD。设计质量(QbD)方法被用作一种强大的策略,可以优化复杂糖分高的食品基质中FD的高通量分析的分析条件。MEPS-方法可操作设计的最佳点:使用R-CX吸附剂,乙腈(ACN)作为洗脱溶剂,三个加载周期和500μL样品体积,获得了区域(MODR)。-1。通过蒙特卡罗仿真和估计残差的能力分析证明了其鲁棒性。所有FD的浓度-响应关系均通过多项式函数模型描述,并通过Fisher方差(F检验)进行了确认。回收率百分比在91.9-112.1%的范围内。观察到良好的方法精度,相对标准偏差(RSD)的可重复性小于4.9%,中等精度的小于8.8%。分析物的定量限为30.6至737.7μgkg -1。MEPS R-CX / UHPLC CORTECS-PDA方法揭示了基于FD的目标分析进行SCH真实性控制的有效且潜在的分析工具,从而可以严格控制和区别于其他相似或掺假的产品。

更新日期:2017-09-08
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