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Validation of an Analytical Method to Determine the Content of Acrylamide in Roasted Coffee

机译:测定烘焙咖啡中丙烯酰胺含量的分析方法的验证

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摘要

An inter-laboratory comparison study was carried out to evaluate the effectiveness of a method that was standardised for the determination of acrylamide in bakery and potato products for the determination of acrylamide in roasted coffee. The intention was to extend the scope of the standardised method to roasted coffee. Therefore only slight modifications of the standardised method were tolerated.The method is based on aqueous extraction of the roasted coffee matrix and solid phase extraction (SPE) clean-up followed by isotope dilution high performance liquid chromatography with tandem mass spectrometric detection (LC-MS/MS). The test portion of the sample was spiked with isotope labelled acrylamide and extracted on a mechanical shaker with n-hexane and water for one hour. The sample extract was centrifuged, the organic phase was discarded, and a portion of the aqueous extract was further cleaned-up by solid phase extraction on Isolute Multimode followed by Isolute ENV+ columns. The acrylamide-containing fraction eluted from the second SPE column was evaporated to about 500 µL and analysed by reverse-phase high performance liquid chromatography (HPLC) with tandem mass spectrometric detection.Three coffee samples and one aqueous acrylamide standard solution (quality control sample) were sent to 11 laboratories from 8 EU Member States. All samples were sent as blinded duplicates.Based on the reported results the relative standard deviations for reproducibility (RSDR) were 11.5 % at an acrylamide level of 160 µg/kg, 10.1 % at a level of 263 µg/kg, and 9.6 % at a level of 585 µg/kg. The values for RSDr in those materials ranged from 1 % to 3.5 %.
机译:进行了实验室间的比较研究,以评估标准化方法用于测定烘焙食品和马铃薯产品中丙烯酰胺的方法,以及测定烘焙咖啡中丙烯酰胺的方法的有效性。目的是将标准化方法的范围扩展到烘焙咖啡。因此,仅允许对标准方法进行少量修改。该方法基于烘焙咖啡基质的水提取和固相萃取(SPE)净化,然后进行同位素稀释高效液相色谱和串联质谱检测(LC-MS) /多发性硬化症)。用同位素标记的丙烯酰胺加标样品的测试部分,并在机械振荡器上用正己烷和水萃取一小时。离心样品提取物,弃去有机相,然后通过在Isolute Multimode上进行固相萃取,然后在Isolute ENV +色谱柱上进一步净化部分水相萃取液。从第二个SPE柱洗脱的含丙烯酰胺馏分蒸发至约500μL,并通过反相高效液相色谱(HPLC)和串联质谱检测进行分析.3个咖啡样品和1个丙烯酰胺标准水溶液(质量控制样品)被送至8个欧盟成员国的11个实验室。所有样品均以盲法重复发送。根据报告的结果,丙烯酰胺含量为160 µg / kg时,相对重现性标准偏差(RSDR)为11.5%,含量为263 µg / kg时为10.1%,含量为9.6%。浓度为585 µg / kg。这些材料中的RSDr值范围为1%至3.5%。

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