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Development and validation of Q-TOF/MS method for the rapid and simultaneous quantification of three aconitum alkaloids in food

机译:快速和同时定量食品中三种乌头生物碱的Q-TOF / MS方法的开发和验证

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摘要

The safety of food is occasionally questionable, as there have been some reports of products contaminated with illegal adulterants. In this study, the presence of three aconitum alkaloids (aconitine, mesaconitine, and hypaconitine) in food was determined by liquid chromatography-tandem mass spectroscopy (LC-MS/MS) and quadruple time of flight mass spectrometry (Q-TOF/MS). The LC-MS/MS method was validated. The linearity (R2) was more than 0.999, and the LODs and LOQs ranged from 0.010 to 0.200 ng mLa?’1 and 0.025 to 0.500 ng mLa?’1, respectively. The precisions were 0.25a€“2.27% (intra-day) and 0.44a€“5.47% (inter-day), and the accuracies were 86.45a€“106.45% (intra-day) and 87.54a€“106.95% (inter-day). The mean recoveries of the spiked samples ranged from 99.04% to 102.30%. The relative standard deviation (RSD) of the stability was less than 7.33%. Using the developed method, the aconitum alkaloids were detected in 10 tested samples, obtained between 2012 and 2014, in the following quantities: aconitine, 57.1%; mesaconitine, 7.1%; and hypaconitine, 7.1%. Monitoring the presence of these three aconitum alkaloids in food should be pursued in the interest of human health, and the results of this study confirm that the developed method will be useful towards that end.
机译:食品安全有时会受到质疑,因为有报告称产品被非法掺假物污染。在这项研究中,通过液相色谱-串联质谱(LC-MS / MS)和四倍飞行时间质谱(Q-TOF / MS)确定了食品中三种乌头生物碱(阿尼尼丁,中阿尼尼丁和猪碱)的存在。 。 LC-MS / MS方法得到验证。线性度(R2)大于0.999,LOD和LOQ分别为0.010至0.200 ng mLa?-1和0.025至0.500 ng mLa?1。精度为0.25a€2.27%(日内)和0.44a€5.47%(日内),精度为86.45a€106.45%(日内)和87.54a€106.95%(日内)日间)。加标样品的平均回收率在99.04%到102.30%之间。稳定性的相对标准偏差(RSD)小于7.33%。使用开发的方法,在2012年至2014年之间获得的10个测试样品中检出乌头生物碱,其含量为:乌头碱57.1%;乌头碱57.1%。美沙尼汀,7.1%;以及尼古丁7.1%为了人类健康的利益,应该对食品中这三种乌头生物碱的存在进行监测,这项研究的结果证实,开发的方法将有助于实现这一目标。

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