Identification of Phylloquinone (Vitamin K1) as an Unknown Peak in Electron Capture Detection Gas Chromatograms of Pyrethroid Insecticide Residues

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Abstract

An unknown peak was observed in spinach extract during routine analysis of 7 pyrethroid insecticides by gas chromatography with electron capture detection (GC-ECD) using a DB-1 column (20 m × 0.25 mm id, 0.1 μm film thickness). It eluted later than the 7 pyrethroids, and it was also found in other agricultural crops. The intensity of the unknown peak was related to the green color of the sample: It was absent in white vegetables such as radish root or onion. Data from GC/direct deposition/Fourier-transform infrared spectroscopy (FTIR) suggested it might be phylloquinone (vitamin K1). The identity was confirmed also by using electron impact capillary GC/mass spectrometry (MS). Although phylloquinone has no halogens, it showed very high sensitivity by ECD (63Ni), responding to 10 pg.

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Imanaka, M., Kadota, M., Kumashiro, K., & Mori, T. (1996). Identification of Phylloquinone (Vitamin K1) as an Unknown Peak in Electron Capture Detection Gas Chromatograms of Pyrethroid Insecticide Residues. Journal of AOAC International, 79(2), 538–543. https://doi.org/10.1093/jaoac/79.2.538

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