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A highly sensitive ultra-high performance liquid chromatography/tandem mass spectrometry method with in-source fragmentation for rapid quantification of raspberry ketone
Journal of Food and Drug Analysis ( IF 3.6 ) Pub Date : 2019-07-01 , DOI: 10.1016/j.jfda.2018.07.005
Bo Yuan 1, 2 , Danyue Zhao 1 , Ruoyuan Du 2 , Dushyant Kshatriya 3 , Nicholas T Bello 3 , James E Simon 1 , Qingli Wu 1, 2
Affiliation  

Raspberry ketone (RK) is the characteristic aromatic compound in raspberry (Rubus idaeus L.) with wide applications as food additive and anti-obesity agent. However, quantification of RK has presented difficulties in MS detection and reliable LC-MS method for RK analysis in literature is in limit to date. In order to facilitate quality control of raspberry derived products and RK metabolomics study, this study aimed to develop a validated and sensitive UHPLC-MS/MS method. Strong in-source fragmentation was noted and the fragmental ion of 107 m/z produced was selected as the precursor ion for MRM detection, and as such the electrospray ionization performance was optimized by fractional factorial design to accommodate such ion-source dissociation behavior as well as its moderate volatility. A pathway involving the formation of quinone-like structure with strong conjugation was proposed to explain the intense in-source fragmentation. The MRM transition was optimized with product ion of 77 m/z selected as the quantifier ion. The method featured low limit of quantification of ~2 ng/mL and allowed for rapid detection of RK in fresh raspberries following direct sample preparation. RK contents were found to be higher from locally grown and harvested farm sources compared to commercial products shipped into the state, and higher in those at late-stage compared with early-stage maturity. No correlations in RK content between organic and non-organic labels were noted.

中文翻译:

一种用于快速定量覆盆子酮的高灵敏度超高效液相色谱/串联质谱法与源内碎裂法

覆盆子酮(RK)是覆盆子(Rubus idaeus L.)中特有的芳香族化合物,广泛用作食品添加剂和抗肥胖剂。然而,RK 的量化在 MS 检测中存在困难,文献中用于 RK 分析的可靠 LC-MS 方法是有限的。为了促进覆盆子衍生产品的质量控制和 RK 代谢组学研究,本研究旨在开发一种经过验证且灵敏的 UHPLC-MS/MS 方法。注意到强烈的源内碎片化,产生的 107 m/z 碎片离子被选为 MRM 检测的前体离子,因此通过部分因子设计优化了电喷雾电离性能以适应这种离子源解离行为作为其温和的波动性。提出了一种涉及形成具有强共轭的类醌结构的途径来解释强烈的源内碎片。选择 77 m/z 的子离子作为定量离子对 MRM 离子对进行了优化。该方法具有约 2 ng/mL 的低定量限,并允许在直接样品制备后快速检测新鲜覆盆子中的 RK。与运入该州的商业产品相比,本地种植和收获的农场来源的 RK 含量被发现更高,并且与早期成熟相比,后期的 RK 含量更高。没有注意到有机和非有机标签之间的 RK 含量的相关性。该方法具有约 2 ng/mL 的低定量限,并允许在直接样品制备后快速检测新鲜覆盆子中的 RK。与运入该州的商业产品相比,本地种植和收获的农场来源的 RK 含量被发现更高,并且与早期成熟相比,后期的 RK 含量更高。没有注意到有机和非有机标签之间的 RK 含量的相关性。该方法具有约 2 ng/mL 的低定量限,并允许在直接样品制备后快速检测新鲜覆盆子中的 RK。与运入该州的商业产品相比,本地种植和收获的农场来源的 RK 含量被发现更高,并且与早期成熟相比,后期的 RK 含量更高。没有注意到有机和非有机标签之间的 RK 含量的相关性。
更新日期:2019-07-01
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