Citation: WANG Siwei, LIU Yanping, SUN Haibin, DU Lanjuan, XU Nengli. Determination of myclobutanil and difenoconazole residues in pollen and honey of litchi by high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2018, 36(1): 17-22. doi: 10.3724/SP.J.1123.2017.09034 shu

Determination of myclobutanil and difenoconazole residues in pollen and honey of litchi by high performance liquid chromatography-tandem mass spectrometry

Institute of Plant Protection Guangdong Academy of Agricultural Sciences, Guangdong Provincial Key Laboratory of High Technology for Plant Protection, Guangzhou 510640, China

Received Date: 20 September 2017

Fund Project: China Litchi and Longan Research System (No. CARS-33-16)

An effective method was developed for the determination of two major fungicides including myclobutanil and difenoconazole residues in pollen and honey of litchi by modified QuEChERS-high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The pollen and honey samples were all extracted by acetonitrile, the pollen samples were cleaned-up by 0.9 g anhydrous magnesium sulfate (MgSO₄), 0.15 g primary secondary amine (PSA) and 0.15 g C₁₈; the honey samples were cleaned-up by 0.9 g MgSO₄ and 0.15 g PSA. The 0.1% (v/v) formic acid aqueous solution-acetonitrile (25:75, v/v) were used as the mobile phases. The extracts were separated on a Poroshell-120 EC-C₁₈ chromatographic column, the positive electrospray ion (ESI⁺) source and selected ion monitoring (SIM) mode were used. The analytes were quantified by the matrix matching standard solutions. The matrix matched standard solutions of myclobutanil and difenoconazole showed good linearities in the range of 1-100 μg/L, and the correlation coefficients (r²) were all above 0.9990. The limits of detection (LODs) of myclobutanil and difenoconazole were 0.25 μg/kg and 0.50 μg/kg, respectively. The limits of quantification (LOQs) of myclobutanil and difenoconazole were 0.83 μg/kg and 1.7 μg/kg, respectively. The average recoveries of myclobutanil and difenoconazole in pollen and honey samples were 87.0%-95.2% and 90.1%-96.4% with the relative standard deviations of 1.2%-3.6% and 0.7%-4.1%, respectively. The method is quick, easy and sensitive, and it is suitable for the rapid determination and trace analysis of myclobutanil and difenoconazole in pollens and honeys of litchi. The method can provide data support for the exposure risk assessment of bees and other pollination insects.
- high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS),
- QuEChERS,
- myclobutanil,
- difenoconazole,
- pollen and honey of litchi
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