Abstract
In this study, dispersive solid phase extraction (DSPE) combined with dispersive liquid–liquid microextraction (DLLME) method was developed for the determination of triazole fungicide residues in tea samples. DSPE with ODS C18, primary secondary amine, and florisil as sorbents was applied to clean up and minimize matrix interference from tea samples; it was followed with the enrichment of target compounds in the DLLME procedure and detection with liquid chromatography–tandem mass spectrometry (LC-MS/MS). The effects of various experimental parameters on the DSPE and DLLME procedures were studied systematically, such as the kinds and volume of sorbents, extraction and dispersive solvents, and extraction time. Under optimum conditions, the method was validated in a tea matrix. The matrix-matched calibration curves of three triazoles had good linearity in the range of 0.0125–50 μg kg−1, and the linear regression coefficients (r) ranged from 0.9998 to 0.9999. The limits of quantification (S/N = 10) for penconazole, tebuconazole, and triadimenfon were 4.0, 7.8, and 31.6 ng kg−1, respectively. The intra-day and inter-day relative standard deviations varied from 3.6 to 18.6 %. Recoveries in three concentration levels were between 91 and 118 %. The obtained results show that the proposed DSPE-DLLME-LC-MS method has the potential to analyze trace fungicides in a complex sample matrix.
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Abbreviations
- DSPE:
-
Dispersive solid phase extraction
- DLLME:
-
Dispersive liquid–liquid microextraction
- LC-MS/MS:
-
Liquid chromatography–tandem mass spectrometry
- RSD:
-
Relative standard deviation
- LOQs:
-
Limits of quantification
- MRLs:
-
Maximum residue limits
- LLE:
-
Liquid–liquid extraction
- SPE:
-
Solid phase extraction
- SPME:
-
Solid phase microextraction
- PSA:
-
Primary secondary amine
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Acknowledgments
The project was supported by National Natural Science Foundation of China (no. 21175052), “Chen Guang” project of Wuhan (no. 201050231065), and Scientific and Technological Brainstorm Project of Wuhan (no. 201060623259).
Conflict of Interest
The authors indicate that they have no financial relationship with the organization that sponsored the research. Hui Xu declares that she has no conflict of interest. Yu Zhang declares that she has no conflict of interest. This article does not contain any studies with human and animal subjects.
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Zhang, Y., Xu, H. Determination of Triazoles in Tea Samples Using Dispersive Solid Phase Extraction Combined with Dispersive Liquid–Liquid Microextraction Followed by Liquid Chromatography–Tandem Mass Spectrometry. Food Anal. Methods 7, 189–196 (2014). https://doi.org/10.1007/s12161-013-9617-5
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DOI: https://doi.org/10.1007/s12161-013-9617-5