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Headspace in-tube microextraction combined with reverse-flow micellar electrokinetic capillary chromatography for detection of pyrethroid herbicides in fruits

Yue Mei-E, Lin Qiaoyan, Xu Jie, Jiang Ting-Fu

Acta Chromatographica

2019

Vol. 31, no. 3

189--193

A rapid, simple, and sensitive method has been developed for the analysis of pyrethroid herbicides in fruits by using headspace in-tube microextraction (HS-ITME) coupled with reverse-flow micellar electrokinetic capillary chromatography (RF-MECC). In the newly developed method, by placing a capillary filled with background electrolyte (BGE) of RF-MECC in the HS above the sample solution, the pyrethroid herbicides were extracted into the acceptor phase in the capillary. After extraction, electrophoresis of the extracts in the capillary was carried out. The influence of some essential BGE components such as sodium dodecyl sulfate (SDS) and organic modifiers concentrations was investigated. Extraction parameters were also systematically investigated, including the extraction temperature, extraction time, salt concentration, and volume of the sample solution. Under the optimized conditions, enrichment factors for three pyrethroids were 309, 133, and 288, respectively. The proposed method provided a good linearity, low limits of detection (below 1.00 ng/mL), and good repeatability of the extractions (relative standard deviations [RSDs] below 7.83%, n = 6). The fruit samples were analyzed by the proposed method, and the obtained results indicated that the proposed method provides acceptable recoveries and precisions.

Simultaneous separation and analysis of two bioactive xanthones in the Tibetan medicinal plant Gentianopsis paludosa (Hook. f.) Ma by micellar electrokinetic capillary chromatography

Cheng Y. Q., Zhang Y. X, Qi S. D., Chen H. L., Chen X. G.

Acta Chromatographica

2010

Vol. 22, no. 4

637--650

1,7-Dihydroxy-3,8-dimethoxyxanthone (X1) and 1,8-dihydroxy-3,7-dimethoxyxanthone (X2) are two important xanthones of the Tibetan medicinal plant Gentianopsis paludosa (Hook. f.) Ma. They are very similar in structure, the only difference being exchange of OH and OCH 3 at the 7 and 8 positions. By calculations based on the geometry of the molecules using the MM+ force field, the different distances between the hydroxyl groups of the two xanthones were obtained (4.64774 Å for X2 and 7.19412 Å for X1), therefore, the two hydroxyl groups of X1 should freely interact with more water molecules than those of X2 in aqueous solution. In other words, X2 is more hydrophobic than X1. Micellar electrokinetic capillary chromatography (MEKC) was therefore chosen for separation of the compounds. The optimum separation conditions were: 20 mM borate + 20 mM SDS (pH 9.8) as running buffer, 17.5 kV applied potential, and detection wavelength 260 nm. The two xanthones were well separated in 9.0 min, with Gaussian peak shapes. The repeatability of the MEKC method (expressed as RSD) for X1 and X2 was 0.9 and 1.1%, respectively, for migration time, and 3.1 and 1.4% for peak area. The limits of detection ( S/N = 3) were 0.41 μg mL -1 for X1 and 0.82 μg mL -1 for X2. The recovery of the MEKC method for the two xanthones was also satisfactory.