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高通量分析方法用于肉类和家禽中的 265 种农药和环境污染物,采用快速低压气相色谱和超高液相色谱串联质谱法。

High-throughput analytical method for 265 pesticides and environmental contaminants in meats and poultry by fast low pressure gas chromatography and ultrahigh-performance liquid chromatography tandem mass spectrometry.

机构信息

U.S. Department of Agriculture, Agricultural Research Service, Eastern Regional Research Center, 600 East Mermaid Lane, Wyndmoor, PA 19038, USA.

出版信息

J Chromatogr A. 2018 Oct 19;1572:203-211. doi: 10.1016/j.chroma.2018.08.025. Epub 2018 Aug 16.

Abstract

A high throughput method for simultaneous determination of 200 pesticides and 65 environmental contaminants: polychlorinated biphenyls (PCBs), polycyclic aromatic hydrocarbons (PAHs), polybrominated diphenyl ethers (PBDEs) and other flame retardants, was developed and validated in cattle, swine and poultry muscle tissues. The method was based on sample preparation with QuEChERS extraction followed by an automated robotic sample cleanup with solid phase extraction (SPE) mini-columns using Instrument Top Sample Preparation (ITSP). The automated robotic ITSP was integrated with instrumental analysis (low pressure (LP)GC-MS/MS) to conduct sample cleanup and analysis in parallel. Another aliquot of the initial QuEChERS extract was subjected to UHPLC-MS/MS analysis, and 53 overlapping pesticides were analyzed by both LPGC- and UHPLC-MS/MS (10 min each). Fit-for-purpose LOQs<5 ng/g were achieved for ≥90% of the analytes. The method was validated in cattle, swine and chicken muscles at three spiking levels at and below the US regulatory levels of concern, and satisfactory recoveries (70-120%) and RSDs ≤ 20% were demonstrated for 219 analytes. Matrix effects were within ±20% for 78-97% of LC- and GC-amenable analytes. The validated method was successfully applied for the analysis of real-world incurred meat and poultry samples, further demonstrating its applicability to real-world samples, and potential for implementation in routine monitoring of contaminants.

摘要

建立并验证了一种高通量方法,用于同时测定牛、猪和禽肌肉组织中的 200 种农药和 65 种环境污染物:多氯联苯(PCBs)、多环芳烃(PAHs)、多溴二苯醚(PBDEs)和其他阻燃剂。该方法基于 QuEChERS 提取的样品制备,然后使用 Instrument Top Sample Preparation(ITSP)自动机器人固相萃取(SPE)小柱进行自动机器人样品净化。自动机器人 ITSP 与仪器分析(低压(LP)GC-MS/MS)集成,用于并行进行样品净化和分析。初始 QuEChERS 提取物的另一份等分试样进行 UHPLC-MS/MS 分析,通过 LPGC-和 UHPLC-MS/MS 分析了 53 种重叠农药(每种 10 分钟)。≥90%的分析物达到了<5 ng/g 的专用 LOQs。该方法在牛、猪和鸡肌肉中三个加标水平进行了验证,加标水平低于美国关注的监管水平,对于 219 种分析物,回收率(70-120%)和 RSD(≤20%)令人满意。对于 78-97%的 LC 和 GC 可分析的分析物,基质效应在±20%以内。该验证方法成功应用于实际发生的肉类和家禽样品的分析,进一步证明了其在实际样品中的适用性,并有可能在污染物的常规监测中实施。

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