关键词: HPLC–QQQ HPLC–QTOF/MS dietary supplements sildenafil derivatives standard‐free detection of adulteration (SFDA)

Mesh : Dietary Supplements / analysis Sildenafil Citrate / analysis Tandem Mass Spectrometry / methods Drug Contamination Chromatography, High Pressure Liquid / methods Reproducibility of Results Limit of Detection Linear Models Phosphodiesterase 5 Inhibitors / analysis

来  源:   DOI:10.1002/bmc.5925

Abstract:
The rapid and accurate detection of illegal adulteration of chemical drugs into dietary supplements is a big challenge in the food chemistry field. Detection of compounds without a standard reference is even more difficult; however, this is a common situation. Here in this study, a novel \"standard-free detection of adulteration\" (SFDA) method was proposed and phosphodiesterase-5 inhibitor derivatives were used as an example to figure out the possibility and reliability of this SFDA method. After analysis by quadrupole coupled time of flight-tandem mass spectrometry detection and multivariable statistics, six common fragment ions were chosen to indicate whether adulteration was present or not, while 20 characteristic fragment ions indicated whether adulteration was by nitrogen-containing heterocycles or by anilines. Furthermore, the quantitative methods were conducted by high-performance liquid chromatography-tandem mass spectrometry. In a word, this strategy allows for a quick determination of dietary supplement adulteration without any need for standard materials, improving the efficacy of food safety testing.
摘要:
快速准确地检测膳食补充剂中非法掺假化学药物是食品化学领域的一大挑战。没有标准参考的化合物的检测更加困难;然而,这是常见的情况。在这项研究中,提出了一种新型的“无标准掺假检测”(SFDA)方法,并以磷酸二酯酶-5抑制剂衍生物为例,以确定该SFDA方法的可能性和可靠性。经过四极耦合飞行时间-串联质谱检测和多变量统计分析,选择了六种常见的碎片离子来表明是否存在掺假,而20个特征性碎片离子表明掺杂是通过含氮杂环还是通过苯胺。此外,采用高效液相色谱-串联质谱进行定量。一句话,这种策略允许快速确定膳食补充剂掺假,而不需要任何标准材料,提高食品安全检测的有效性。
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