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Sensitive determination of carbamates in fruit and vegetables by a combination of solid-phase extraction and dispersive liquid-liquid microextraction prior to HPLC

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Abstract

We report on a new method for sample pretreatment. It is based on solid-phase extraction combined with dispersive liquid-liquid microextraction (SPE-DLLME) and was applied to the determination of carbamates in apple and cucumber. The carbamates carbofuran, carbaryl, and pirimicarb were first extracted from samples by SPE. The analytes were then eluted from the sorbent with acetonitrile, and the DLLME technique was then applied to the resulting eluate. Finally, the analytes in the extraction solvent were determined by HPLC. Several parameters affecting the SPE-DLLME process were optimized. The new method provides enrichment factors that range from 5,400 to 7,650. Calibration plots are linear in the range from 0.25 to 100 μg kg−1 for carbofuran and carbaryl, and from 0.10 to 100 μg kg−1 for pirimicarb, with correlation coefficient (r2) ranging from 0.9980 to 0.9997. The limits of detection range from 5 to 60 pg kg−1 (at S/N = 3). The method was successfully applied to the extraction and sensitive determination of carbamates in apple and cucumber samples.

Chromatograms of non-spiked apple sample with the treatment of SPE-DLLME (1), apple sample spiked with carbamates at the concentration of 10.0 μg kg-1 without (2) / with (3) the treatment of SPE-DLLME.

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Acknowledgements

This work was supported by Education Department of Hubei Province (grant no. T201101), the National Nature Science Foundation of China (grant no. 20975030, 20835004), the Natural Science Foundation of Hubei province of China (grant no. 2009CDB364), and the Specialist Fund of Hubei University (020091130-ky2006004). The authors would like to thank their colleagues for their valuable technical assistance.

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  1. College of Chemistry and Chemical Engineering, Hubei University, Wuhan, 430062, China

    Shu Zhou, Huaixia Chen, Bo Wu, Chao Ma & Yong Ye

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  1. Shu Zhou
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  2. Huaixia Chen
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  3. Bo Wu
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  4. Chao Ma
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Correspondence to Huaixia Chen.

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Zhou, S., Chen, H., Wu, B. et al. Sensitive determination of carbamates in fruit and vegetables by a combination of solid-phase extraction and dispersive liquid-liquid microextraction prior to HPLC. Microchim Acta 176, 419–427 (2012). https://doi.org/10.1007/s00604-011-0735-8

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  • DOI: https://doi.org/10.1007/s00604-011-0735-8

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