2013•Chinese Journal of ChromatographyRequires access

Determination of 11 triazole fungicides in fruits using solid phase extraction and gas chromatography-tandem mass spectrometry

Jige Li, Yufei Wang, Jiawei Shi, Jiang Li, Xunping Yao, Lanyun Fang

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Abstract

A method was developed and validated for the simultaneous determination of 11 triazole fungicides (tetraconazole, triflumizole, penconazole, hexaconazole, flutriafol, myclobutanil, etuconazole, propiconazole, tebuconazole, epoxiconazole and fluquinconazole) in fruits by gas chromatography-tandem mass spectrometry (GC-MS/MS). The triazole fungicides were extracted from the samples with acetonitrile, then enriched and cleaned-up with solid phase extraction (SPE) on a Carbon/NH2 cartridge (collecting 2 - 10 mL effluent). The detection was carried out by GC-MS/MS in the multiple reaction monitoring (MRM) mode, and the quantification analysis was performed by external standard method. The calibration curves showed good linearity in the range of 10 - 500 microg/L. The correlation coefficients were larger than 0. 994 0. The average recoveries of the 11 fungicides spiked in the fruits at the levels of 10, 50, 100 and 250 microg/kg were between 82.6% and 117.1%, and the relative standard deviations (RSD) were less than 10%. The limits of quantification (S/N = 10) were between 0.8 microg/kg and 3.4 microg/kg. The method possesses low background, high sensitivity, and quantification limits lower than that of the national standard and the values reported in the relevant literature. It can be applied to the routine analysis of the 11 triazole fungicides in fruits.

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What this paper is about

A method was developed and validated for the simultaneous determination of 11 triazole fungicides (tetraconazole, triflumizole, penconazole, hexaconazole, flutriafol, myclobutanil, etuconazole, propiconazole, tebuconazole, epoxiconazole and fluquinconazole) in fruits by gas chromatography-tandem mass spectrometry (GC-MS/MS). The triazole fungicides were extracted from the samples with acetonitrile, then enriched and cleaned-up with solid phase extraction (SPE) on a Carbon/NH2 cartridge (collecting 2 - 10 mL effluent). The detection was carried out by GC-MS/MS in the multiple reaction monitoring (MRM) mode, and the quantification analysis was performed by external standard method. The calibration curves showed good linearity in the range of 10 - 500 microg/L. The correlation coefficients were larger than 0. 994 0. The average recoveries of the 11 fungicides spiked in the fruits at the levels of 10, 50, 100 and 250 microg/kg were between 82.6% and 117.1%, and the relative standard deviations (RSD) were less than 10%. The limits of quantification (S/N = 10) were between 0.8 microg/kg and 3.4 microg/kg. The method possesses low background, high sensitivity, and quantification limits lower than that of the national standard and the values reported in the relevant literature. It can be applied to the routine analysis of the 11 triazole fungicides in fruits.

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Available abstract

A method was developed and validated for the simultaneous determination of 11 triazole fungicides (tetraconazole, triflumizole, penconazole, hexaconazole, flutriafol, myclobutanil, etuconazole, propiconazole, tebuconazole, epoxiconazole and fluquinconazole) in fruits by gas chromatography-tandem mass spectrometry (GC-MS/MS). The triazole fungicides were extracted from the samples with acetonitrile, then enriched and cleaned-up with solid phase extraction (SPE) on a Carbon/NH2 cartridge (collecting 2 - 10 mL effluent). The detection was carried out by GC-MS/MS in the multiple reaction monitoring (MRM) mode, and the quantification analysis was performed by external standard method. The calibration curves showed good linearity in the range of 10 - 500 microg/L. The correlation coefficients were larger than 0. 994 0. The average recoveries of the 11 fungicides spiked in the fruits at the levels of 10, 50, 100 and 250 microg/kg were between 82.6% and 117.1%, and the relative standard deviations (RSD) were less than 10%. The limits of quantification (S/N = 10) were between 0.8 microg/kg and 3.4 microg/kg. The method possesses low background, high sensitivity, and quantification limits lower than that of the national standard and the values reported in the relevant literature. It can be applied to the routine analysis of the 11 triazole fungicides in fruits.

Key concepts: Myclobutanil, Tebuconazole, Chemistry, Chromatography, Gas Chromatography/Tandem Mass Spectrometry, Hexaconazole, Pyrimethanil, Solid phase extraction

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