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J Agric Food Chem. 2015 May 13;63(18):4457-63. doi: 10.1021/jf5056248. Epub 2015 Jan 16.

High-throughput simultaneous analysis of pesticides by supercritical fluid chromatography coupled with high-resolution mass spectrometry.

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†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.


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).


SFC/MS; high-resolution mass spectrometry; high-throughput analysis; identification criteria; multiresidue; pesticide

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