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借助液相色谱-线性离子阱质谱联用仪(LC-LIT-MS)和液相色谱-四极杆飞行时间质谱联用仪(LC-Q-TOF-MS),通过替代沉淀途径对谷物中的串珠镰刀菌素进行定量评估。

Quantitative assessment of moniliformin in cereals via alternative precipitation pathways, aided by LC-LIT-MS and LC-Q-TOF-MS.

作者信息

Lim Chee Wei, Lai Kit Yee, Yeo Jie Fang, Tai Siew Hoon, Chan Sheot Harn

机构信息

Food Safety Laboratory, Applied Sciences Group, Health Sciences Authority, 11 Outram Road, Singapore 169078, Singapore.

Food Safety Laboratory, Applied Sciences Group, Health Sciences Authority, 11 Outram Road, Singapore 169078, Singapore.

出版信息

Food Chem. 2015 May 1;174:372-9. doi: 10.1016/j.foodchem.2014.11.069. Epub 2014 Nov 15.

Abstract

The availability of a simple chemical precipitation workflow aided by targeted and untargeted mass spectrometry would provide an accurate diagnostic platform for the direct determination of moniliformin in cereals for food safety control. In-house method validation was performed at six concentration levels of 8, 40, 80, 200, 400, and 600 ng g(-1) in cereal flours of wheat, corn, rye, oats and barley. Spiking experiments were made at three concentration levels of 20, 40 and 100 ng g(-1). Protein precipitation and "PHREE" column cleanup strategy provided recoveries of 81-108% for all cereals matrices using external calibrants. "PHREE" purification provided significant (p < 0.05) ion signal enhancement reduction advantage for all matrices except corn flour. Moniliformin underwent significant (p < 0.05) degradation over 2 weeks when prepared in acidified water. A simple, low-cost and fit-for-purpose procedure for the identification and quantitation of moniliformin in cereals becomes available to support prospective regulatory function.

摘要

借助靶向和非靶向质谱的简单化学沉淀工作流程,可为食品安全控制直接测定谷物中的串珠镰刀菌素提供一个准确的诊断平台。在小麦、玉米、黑麦、燕麦和大麦的谷物粉中,在8、40、80、200、400和600 ng g(-1) 这六个浓度水平上进行了内部方法验证。在20、40和100 ng g(-1) 这三个浓度水平上进行了加标实验。蛋白质沉淀和“PHREE”柱净化策略使用外部校准物时,所有谷物基质的回收率为81-108%。“PHREE”净化除了玉米粉外,对所有基质都提供了显著(p < 0.05)的离子信号增强降低优势。串珠镰刀菌素在酸化水中制备时,在2周内发生了显著(p < 0.05)降解。一种用于鉴定和定量谷物中串珠镰刀菌素的简单、低成本且适用的方法可用于支持前瞻性监管功能。

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