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Use of chiral derivatization for the determination of dichlorprop in tea samples by ultra performance LC with fluorescence detection
Author(s) -
Inoue Koichi,
Prayoonhan Nuntawat,
Tsutsui Haruhito,
Sakamoto Tasuku,
Nishimura Maiko,
Toyo'oka Toshimasa
Publication year - 2013
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201201187
Subject(s) - chromatography , derivatization , enantiomer , chemistry , repeatability , formic acid , high performance liquid chromatography , calibration curve , detection limit , organic chemistry
Dichlorprop is available for agricultural use as a chiral pesticide. In this study, the stereoselective determination of dichlorprop enantiomers in tea samples such as green, black, jasmine, and oolong was developed by ultra performance LC with fluorescence spectrometry after covalent chiral derivatization. The separation was achieved on an Acquity BEH C 18 column with the mobile phase consisting of 0.1% formic acid in acetonitrile/water at a flow rate of 0.4 mL/min. In the covalent chiral derivatization using ( S )‐(+)‐4‐( N , N ‐dimethylaminosulfonyl)‐7‐(3‐aminopyrrolidin‐1‐yl)‐2,1,3‐benzoxadiazole, the peak resolution between the S and R ‐dichlorprop enantiomers was 2.6. LOD s and LOQ s values were 10 and 50 ng/mL standard solution. The linearity of the calibration curves yielded the coefficients ( r 2 > 0.99, ranging from 0.05 to 5 μg/mL) of determination of each of the dichlorprop enantiomers. SPE extraction was used for the sample preparation of dichlorprop in various tea samples. Recoveries were in the range of 82.4–97.6% with associated precision values (within‐day: 82.4–95.8%, n = 6, and between‐day: 83.7–97.6% for 3 days) for repeatability and reproducibility. Based on this result, our method has been proven to be highly efficient and suitable for the routine assay of dichlorprop enantiomers in various tea samples. We propose that the ultra performance LC assay after covalent chiral derivatization would be the renewed tools in the era of chiral stationary platform for chiral pesticide residues in foods.