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Combination of On-Line Solid-Phase Extraction with LC-MS for the Determination of Potentially Hazardous Glycoalkaloids in Potato Products

机译:在线固相萃取与LC-MS联用测定马铃薯产品中潜在的有害糖类生物碱

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A simple and rapid method for the determination of naturally occurring, potentially hazardous glycoalkaloids (GAs) in potatoes and their products has been developed. The procedure is based on the on-line solid-phase extraction of the acetic acid extracts from potato products and combined with liquid chromatography (LC)-mass spectrometry (MS) in a fully automated system (Symbiosis™, Spark Holland Instruments, Emmen, The Netherlands). As sorbent material HySphere™ 18HD was used for alkaloid enrichment. GAs were eluted with the LC gradient and directly analysed by MS. Detection of the analytes was achieved in the sensitive multiple reaction monitoring mode using two characteristic ions (m/z 98 as a qualifier for GAs and m/z 868.3 as a quantifier for α-solanine or m/z 852.4 for α-chaconine). Typical validation data for method precision (v k α-solanine = 5.3–6.5, v k α-chaconine = 3.4–15.4), accuracy (average recovery of α-solanine = 84%, average recovery of α-chaconine = 87%) and linearity over the range from 1 to 1,000 ng ml−1 (R 2 = 0.9915 for α-solanine, R 2 = 0.9939 for α-chaconine) with detection limits of 0.3 ng ml−1 for α-chaconine and 0.5 ng ml−1 for α-solanine were obtained. GA contents of commercial potato products were determined by the new on-line method and afterwards compared with those obtained with an established high-performance LC routine procedure. Better performance of the on-line procedure was obvious from the standard deviations of both methods. Other advantages included a strong reduction of overall analysis time, human intervention and solvent consumption as well as waste production. The time required for the on-line analysis was 5 min, which would allow processing of almost 100 samples in 8 h. Keywords Glycoalkaloids - On-line solid-phase extraction - Potato products - Solanum tuberosum - Solid-phase extraction
机译:已经开发了一种简单快速的方法来测定马铃薯及其产品中天然存在的,潜在有害的糖类生物碱(GAs)。该程序基于从马铃薯产品中提取的乙酸的在线固相萃取,并在全自动系统(Symbiosis™,Spark Holland Instruments,Emmen,荷兰人)。 HySphere™18HD作为吸附剂材料用于生物碱富集。 GAs用LC梯度洗脱并通过MS直接分析。使用两个特征离子(m / z 98作为GAs的定量限,m / z 868.3作为α-茄碱的定量限或m / z 852.4作为α-chaconine的定量限)在灵敏的多反应监测模式下完成了分析物的检测。方法精度(v k α-茄碱= 5.3–6.5,v k α-查茄碱= 3.4-15.4),准确性(α-茄碱的平均回收率)的典型验证数据= 84%,α-查茄碱的平均回收率= 87%)和1到1,000 ng ml -1 范围内的线性(α-茄碱的R 2 = 0.9915) ,对于α-查茄碱,R 2 = 0.9939),对于α-查茄碱的检出限为0.3 ng ml -1 ,对于0.5 ng ml -1 获得α-茄碱。通过新的在线方法确定商品马铃薯产品中的GA含量,然后将其与通过已建立的高性能LC常规程序获得的含量进行比较。从这两种方法的标准偏差来看,在线程序的更好性能是显而易见的。其他优点包括大大减少了总体分析时间,人工干预和溶剂消耗以及废物产生。在线分析所需的时间为5分钟,这将允许在8小时内处理近100个样品。糖生物碱-在线固相萃取-马铃薯产品-马铃薯-固相萃取

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