HPLC–QTOF/MS

  • 文章类型: Journal Article
    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。
    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.
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  • 文章类型: Comparative Study
    Steroidal saponins, which exhibit multiple pharmacological effects, are the major bioactive constituents in herbal medicines from Dioscoreae species. In this study, a sensitive method based on high performance liquid chromatography-mass spectrometry (HPLC-MS) was established and validated for qualitative and quantitative analysis of steroidal saponins in four Dioscoreae herbs including Dioscoreae Nipponica Rhizome (DNR) and Dioscoreae Hypoglaucae Rhizome (DHR), Dioscoreae Spongiosae Rhizome (DSR) and Dioscoreae Rhizome (DR). A total of eleven steroidal saponins were identified by high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (HPLC-QTOF/MS). Furthermore, seven major steroidal saponins was simultaneous quantified using a high performance liquid chromatography coupled with triple quadrupole mass spectrometry (HPLC-QQQ/MS). The qualitative and quantitative analysis results indicated that the chemical composition of DNR, DHR and DSR samples exhibited a high level of global similarity, while the ingredients in DR varied greatly from the other three herbs. Moreover, principal component analysis (PCA) and hierarchical clustering analysis (HCA) were performed to compare and discriminate the Dioscoreae herbs based on the quantitative data. The results demonstrated the qualitative and quantitative analysis of steroidal saponins based on HPLC-MS is a feasible method for quality control of Dioscoreae herbs.
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  • 文章类型: Journal Article
    柑橘(CF),田中柑橘(CWT)或柑橘(CML)的成熟果实,是一种重要的柑橘副产品,具有促进健康和营养的特性。本研究比较了CWT和CML的化学和生物学差异。薄层色谱法和高效液相色谱法,结合四极杆飞行时间串联质谱技术,用于比较CWT和CML的化学概况。总共鉴定了25种化合物,结果表明两种CF物种之间的化学组成存在显着差异。通过高效液相色谱结合二极管阵列检测器方法获得的定量结果表明,柚皮苷在CWT中的含量最高,而nomilin是CML中最主要的成分。还发现CWT具有明显高于CML的自由基清除活性。
    Citri Fructus (CF), the mature fruit of Citrus wilsonii Tanaka (CWT) or Citrus medica L. (CML), is an important citrus by-product with health promoting and nutritive properties. The present study compares the chemical and biological differences of CWT and CML. Thin layer chromatography and high performance liquid chromatography, coupled with quadrupole time-of-flight tandem mass spectrometry techniques, were employed to compare the chemical profiles of CWT and CML. A total of 25 compounds were identified and the results indicated that there were significant differences in chemical composition between the two CF species. The quantitative results obtained by HPLC coupled with diode array detector method demonstrated that naringin was present in the highest amounts in CWT, whilst nomilin was the most dominant constituent in CML. It was also found that CWT had significantly higher free radical-scavenging activity than CML.
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