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首页> 外文期刊>Bulletin of the Korean Chemical Society >Development of Isotope Dilution-Liquid Chromatography/Tandem Mass Spectrometry as a Candidate Reference Method for the Determination of Acrylamide in Potato Chips
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Development of Isotope Dilution-Liquid Chromatography/Tandem Mass Spectrometry as a Candidate Reference Method for the Determination of Acrylamide in Potato Chips

机译：同位素稀释液色谱/串联质谱法作为测定马铃薯片中丙烯酰胺的候选参考方法的发展

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摘要

An isotope dilution-liquid chromatography/tandem mass spectrometric method was developed as a candidate reference method for the accurate determination of acrylamide in potato chips, starch-rich foodstuff cooked at high temperature. Sample was spiked with ~(13)C_3-acrylamide and then extracted with water. The extract was further cleaned up with an Oasis HLB solid-phase extraction (SPE) cartridge and an Oasis mixed-phase cation exchange (MCX) SPE cartridge. The extract was analyzed by using LC/ESI/Tandem MS in positive ion mode. LC with a medium reversed-phase (C4) column was optimized to obtain adequate chromatographic retention and separation of acrylamide. MS was operated to selectively monitor [M+H]~+ ions of the analyte and its isotope analogue at m/z 72 and m/z 75, respectively. Sample was also analyzed by the LC/MS with selectively monitoring the collisionally induced dissociation channels of m/z 72 -> m/z 55 and m/z 75 -> 58. Compared to the LC/MS chromatograms, the LC/MS/MS chromatograms showed substantially reduced background chemical noises coming from solvent clusters formed during ESI spray processes and interferences from sample matrix. Repeatability and reproducibility studies showed that the LC/MS/MS method is a reliable and reproducible method which can provide a typical method precision of 1.0% while the LC/MS results are influenced by chemical interferences.
机译：开发了一种同位素稀释-液相色谱/串联质谱法作为候选参考方法，用于准确测定高温烹煮的马铃薯片，富含淀粉的食品中的丙烯酰胺。样品中加入〜（13）C_3-丙烯酰胺，然后用水萃取。提取物用Oasis HLB固相萃取（SPE）柱和Oasis混合相阳离子交换（MCX）SPE柱进一步净化。通过使用LC / ESI / Tandem MS以正离子模式分析提取物。优化了具有中等反相（C4）色谱柱的LC，以获得足够的色谱保留率和丙烯酰胺分离效果。使用MS分别在m / z 72和m / z 75处选择性地监测分析物及其同位素类似物的[M + H]〜+离子。还通过LC / MS分析样品，并选择性地监测碰撞诱导的解离通道m / z 72-> m / z 55和m / z 75->58。与LC / MS色谱图相比，LC / MS / MS色谱图显示，由于ESI喷涂过程中形成的溶剂簇和样品基质的干扰，本底化学噪音大大降低了。重复性和重现性研究表明，LC / MS / MS方法是一种可靠且可重现的方法，可提供1.0％的典型方法精度，同时LC / MS结果受化学干扰的影响。

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