Validation of the QuEChERSER Method for 245 Pesticides and Environmental Contaminants in Barley and Hemp by Low-Pressure GC: Comparison of Triple Quadrupole MS/MS and Orbitrap HRMS for Qualitative and Quantitative Analysis.

Nicolás Michlig, Steven J Lehotay
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Abstract

Background: Monitoring labs are a fundamental link in the food safety chain, and regulatory demands in a competitive economy call for analytical methods that are simpler, faster, more rugged, and broader in scope. The QuEChERSER mega-method introduced in 2021 meets these monitoring needs, which includes high sample throughput, automated cleanup of extracts, and fast low-pressure gas chromatography (LPGC).

Objective: The goal of this work was to extend the QuEChERSER method to additional matrices and more analytes using LPGC, including comparison of the analytical performances of two different mass spectrometric (MS) analyzers: triple quadrupole tandem MS/MS and orbital ion trap (orbitrap) high-resolution (HR)MS.

Methods: The QuEChERSER mega-method was validated for 245 pesticides and environmental contaminants in barley grains and hemp pellets using automated instrument top sample preparation (ITSP) coupled with LPGC-MS/MS or LPGC-HRMS (orbitrap).

Results: Targeted MS/MS detection proved to be more sensitive than orbitrap using full data acquisition, leading to lower limits of quantification (LOQs) with more analytes yielding acceptable recoveries (70-120%) and repeatabilities (RSDs <20%). In barley, 89% of the compounds met validation criteria in MS/MS and 74% in HRMS, which in hemp were 81% and 66%, respectively. Qualitatively, orbitrap HRMS yielded 1% false positives compared to 3-4% in MS/MS, but due to the higher LOQs, the rates of false negatives were 14-17% in orbitrap vs. 6-10% in MS/MS for the different matrices.

Conclusion: The QuEChERSER mega-method including ITSP+LPGC coupled with MS/MS or orbitrap analysis is a robust approach for multiple applications. In the comparison, MS/MS outperformed the orbitrap in terms of sensitivity, but the orbitrap advantages of easier method development, greater selectivity, and possibility for nontargeted/retrospective analysis permit even broader expansion of analytical scope in the future.

Highlights: ITSP+LPGC- MS/MS or HRMS (orbitrap) analysis as part of the QuEChERSER mega-method is a useful and efficient way to monitor for contaminants in foods.

利用低压气相色谱验证大麦和大麻中 245 种农药和环境污染物的 QuEChERSER 方法:三重四极杆 MS/MS 与 Orbitrap HRMS 在定性和定量分析方面的比较。
背景:监测实验室是食品安全链中的一个基本环节,在竞争激烈的经济环境中,监管要求分析方法更简单、更快速、更坚固耐用、范围更广。2021 年推出的 QuEChERSER 大型方法满足了这些监测需求,其中包括高样品通量、提取物自动净化和快速低压气相色谱法(LPGC):这项工作的目标是利用 LPGC 将 QuEChERSER 方法扩展到更多的基质和更多的分析物,包括比较两种不同质谱分析仪的分析性能:三重四极杆串联质谱/质谱和轨道离子阱(orbitrap)高分辨率质谱:方法:使用自动化仪器顶部样品制备 (ITSP),结合 LPGC-MS/MS 或 LPGC-HRMS(orbitrap),对大麦粒和大麻颗粒中的 245 种农药和环境污染物进行了 QuEChERSER 大型方法验证:目标 MS/MS 检测被证明比使用全数据采集的 orbitrap 更灵敏,从而降低了定量限 (LOQ),更多的分析物获得了可接受的回收率(70-120%)和重复性(RSD):QuEChERSER 大方法包括 ITSP+LPGC 与 MS/MS 或 orbitrap 分析,是一种适用于多种应用的可靠方法。在比较中,MS/MS 在灵敏度方面优于 orbitrap,但 orbitrap 具有方法开发更容易、选择性更强以及可进行非靶标/回顾性分析等优点,因此将来可以扩大分析范围:作为 QuEChERSER 大方法的一部分,ITSP+LPGC- MS/MS 或 HRMS(orbitrap)分析是监测食品中污染物的有效方法。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
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