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首页> 外文期刊>Journal of Agricultural and Food Chemistry >Development and Validation of Quantitative Ultraperformance Liquid Chromatography–Tandem Mass Spectrometry Assay for Anticoagulant Rodenticides in Liver
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Development and Validation of Quantitative Ultraperformance Liquid Chromatography–Tandem Mass Spectrometry Assay for Anticoagulant Rodenticides in Liver

机译：肝脏抗凝血腺体的定量超细液相色谱 - 串联质谱法的发展与验证

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src="http://pubs.acs.org/appl/literatum/publisher/achs/journals/content/jafcau/2017/jafcau.2017.65.issue-31/acs.jafc.7b02280/20170803/images/medium/jf-2017-02280b_0003.gif">Anticoagulant rodenticides (ARs) are used to control rodent populations; however, exposure to nontarget animals occurs. A sensitive and rugged quantitative method was developed, optimized, and validated for eight ARs in liver. Target analytes comprised two chemical classes: hydroxycoumarins (warfarin, coumachlor, dicoumarol, bromadiolone, brodifacoum, and difethialone) and indanediones (diphacinone and chlorophacinone). In this method, liver extracts were cleaned using dispersive solid phase extraction (d-SPE) to remove matrix interferences and analyzed by reverse phase ultraperformance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS). Electrospray ionization in negative ion mode combined with multiple reaction monitoring (MRM) using a triple quadrupole mass spectrometer provided simultaneous confirmation and quantitation. Detection limits spanned 0.75–25 ng/g, and lower quantitation limits were established as 50 ng/g. Interassay method accuracy ranged from 92 to 110% across the analytical range (50–2500 ng/g) using matrix-matched calibrants with good repeatability (relative standard deviations 2–16%). Successful method transfer to another laboratory utilizing an Orbitrap mass analyzer, providing high mass accuracy, was assessed by good method reproducibility during blinded study analyses (6–29%; Horwitz ratios (HORRAT) ≤ 1.5).
机译：src =“http://pubs.acs.org/appl/literatum/publisher/achs/journals/content/jafcau/2017/jafcau.2017.65.issue-31/acs.jafc.7b022280/20170803/images/medium / jf-2017-02280b_0003.gif“andanticoagulant agenticides（ars）用于控制啮齿动物群体;然而，发生暴露于非易胃动物。开发，优化并验证了敏感和坚固的定量方法，验证了肝脏八个AR。靶分析物包含两种化学类别：羟基草林（Warfarin，Coumachlor，Dicoumarol，Bromadiolone，Brodifacoum和Difethialone）和吲哚（二白菜和氯丙酮）。在该方法中，使用分散固相萃取（D-SPE）清洁肝提取物，以除去基质干扰，并通过反相超细液相色谱 - 串联质谱（UPLC-MS / MS）分析。负离子模式中的电喷雾电离结合多重反应监测（MRM）使用三重四极杆质谱仪提供了同时确认和定量。检测限截止0.75-25 ng / g，并将较低的定量限制建立为50ng / g。使用具有良好重复性的矩阵匹配的校准物（相对标准偏差2-16％），绕组方法精度范围为分析范围（50-2500 ng / g）的92至110％。通过在盲目的研究分析中的良好方法再现性评估通过偏心的研究分析（6-29％; Horlwitz比（惊人）≤1.5）通过良好的方法转移到另一个实验室提供高度质量分析仪的另一个实验室的转移。

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