†Department of Biotechnology, Graduate School of Engineering, Osaka University, 2-1 Yamadaoka, Suita, Osaka 565-0871, Japan.
§Miyazaki Agricultural Research Institute, 5805 Shimonaka, Sadowara-cho, Miyazaki 880-0212, Japan.
J Agric Food Chem. 2015 May 13;63(18):4457-63. doi: 10.1021/jf5056248. Epub 2015 Jan 16.
Recently, a generally applicable screening method for multiresidue pesticide analysis, which is simple, quick, and accurate and has a reliable performance, is becoming increasingly important for food safety and international trade. This paper proposes a high-throughput screening methodology that enables the detection of multiresidue pesticides using supercritical fluid chromatography coupled to a high-performance benchtop quadrupole Orbitrap mass spectrometry (SFC/Q Exactive) and an automated library-based detection. A total of 444 chemicals covering a wide polarity range (logPow from -4.2 to 7.7) and a wide molecular weight range (from 99.0 to 872.5) were analyzed simultaneously through a combination of high mass resolution (a value of m/Δm = 70000), high mass accuracy (<5 ppm) with positive/negative polarity switching, and highly efficient separation by SFC. A total of 373 pesticides were detected in QuEChERS spinach extracts without dispersive solid phase extraction at the 10 μg kg(-1) level (provisional maximum residue limits in Japan). In conclusion, the developed analytical system is a potentially useful tool for practical multiresidue pesticide screening with high throughput (time for data acquisition, 72 samples per day; and time for data processing of 72 samples, approximately 45 min).
最近，一种普遍适用于多残留农药分析的筛选方法，因其简单、快速、准确且性能可靠，在食品安全和国际贸易中变得越来越重要。本文提出了一种高通量筛选方法，可使用超临界流体色谱与高性能台式四极轨道阱质谱（SFC/Q Exactive）和基于自动库的检测相结合来检测多残留农药。总共分析了 444 种化学物质，涵盖了广泛的极性范围（logPow 从-4.2 到 7.7）和广泛的分子量范围（从 99.0 到 872.5），通过高质量分辨率（m/Δm = 70000）、正负极性切换时的高质量精度（<5 ppm）以及 SFC 的高效分离相结合。在 QuEChERS 菠菜提取物中，无需分散固相萃取，即可在 10μgkg(-1)的水平（日本暂定最大残留限量）下检测到 373 种农药。总之，开发的分析系统是一种具有高通量（每天采集 72 个样品的时间；处理 72 个样品的数据的时间约为 45 分钟）的实用多残留农药筛选的潜在有用工具。
