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Dispersive liquid–liquid microextraction based on the solidification of a floating organic droplet for simultaneous analysis of diethofencarb and pyrimethanil in apple pulp and peel

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Abstract

A method for analysis of diethofencarb and pyrimethanil in apple pulp and peel was developed by using dispersive liquid–liquid microextraction based on solidification of a floating organic droplet (DLLME-SFO) and high-performance liquid chromatography with diode-array detection (HPLC–DAD). Acetonitrile was used as the solvent to extract the two fungicides from apple pulp and peel, assisted by microwave irradiation. When the extraction process was finished, the target analytes in the extraction solvent were rapidly transferred from the acetonitrile extract to another extraction solvent (1-undecanol) by using DLLME-SFO. Because of the lower density of 1-undecanol than that of water, the finely dispersed droplets of 1-undecanol collected on the top of aqueous sample and solidified at low temperature. Meanwhile, the tiny particles of apple cooled and precipitated. Recovery was tested for a concentration of 8 μg kg−1. Recovery of diethofencarb and pyrimethanil from apple pulp and peel was in the range 83.5–101.3%. The repeatability of the method, expressed as relative standard deviation, varied between 4.8 and 8.3% (n = 6). Detection limits of the method for apple pulp and peel varied from 1.2–1.6 μg kg−1 for the two fungicides. Compared with conventional sample preparation, the method has the advantage of rapid speed and simple operation, and has high enrichment factors and low consumption of organic solvent.

Chromatogram of apple pulp (a) and spiked apple pulp (b) at the concentration level of 0.4 μg g−1 for two fungicides obtained by using DLLME-SFO combined with HPLC-DAD. Peak identification: 1-Diethofencarb, 2- Pyrimethanil

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Acknowledgement

The authors would like to thank the National Natural Science Foundation of China (30971948) and Wuhan’s program for tackling key problems in science and technology (200760423155) for financial support for this work.

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Authors and Affiliations

  1. Key Laboratory of Pesticide and Chemical Biology of the Ministry of Education, College of Chemistry, Central China Normal University, Wuhan, 430079, China

    YiWen Zhou, Jing Cheng, Feng Guo, XiaoRan Zhi & HaiLi Hu

  2. Traditional Chinese Medicine Resource and Compound Prescription of the Ministry of Education, Hubei University of Chinese Medicine, Wuhan, 430065, China

    LinTao Han & Gang Chen

Authors
  1. YiWen Zhou
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  2. LinTao Han
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  3. Jing Cheng
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  4. Feng Guo
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  5. XiaoRan Zhi
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  6. HaiLi Hu
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  7. Gang Chen
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Correspondence to Jing Cheng or Gang Chen.

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YiWen Zhou and LinTao Han are co-first authors.

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Zhou, Y., Han, L., Cheng, J. et al. Dispersive liquid–liquid microextraction based on the solidification of a floating organic droplet for simultaneous analysis of diethofencarb and pyrimethanil in apple pulp and peel. Anal Bioanal Chem 399, 1901–1906 (2011). https://doi.org/10.1007/s00216-010-4567-x

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  • DOI: https://doi.org/10.1007/s00216-010-4567-x

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