Liquid chromatographic methods for the determination of vildagliptin in the presence of its synthetic intermediate and the simultaneous determination of pioglitazone hydrochloride and metformin hydrochloride.

Spencer S Walse, Hakan Karaca

文献索引：Int. J. Biomed. Sci. 7(3) , 201-8, (2011)

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摘要

Ozone fumigation was explored as a means for degrading organic fungicide residues on fresh produce. Fungicides sorbed onto model abiotic glass surfaces or onto grape berries were fumigated separately in a flow-through chamber. Gaseous ozone at a constant concentration of 150 ± 10 ppmv (μL·L(-1)) selectively oxidized fungicides sorbed to model surfaces. Over 140 min, boscalid and iprodione levels did not change significantly based on a single-factor analysis of variance (ANOVA) at the 95% level of confidence (p = 0.05); however, pseudo-first-order losses resulted in observable rate constants of ozonolysis, k(ozonolysis) (min(-1)), of 0.0233 ± 0.0029 (t(1/2) ≈ 29.7 min), 0.0168 ± 0.0028 (t(1/2) ≈ 41.3 min), and 0.0127 ± 0.0010 (t(1/2) ≈ 54.6 min) for fenhexamid, cyprodinil, and pyrimethanil, respectively. The relative degradation of fungicides on berries at gaseous ozone concentrations of 900 ± 12 ppmv (μL·L(-1)) over 2 h was similar to that on glass; decreases in residue concentration were observed for only fenhexamid (∼ 64%), cyprodinil (∼ 38%), and pyrimethanil (∼ 35%) with corresponding k(ozonolysis) (min(-1)) of 0.0085 ± 0.0021 (t(1/2) ≈ 81.5 min), 0.0039 ± 0.0008 (t(1/2) ≈ 177.7 min), and 0.0036 ± 0.0007 (t(1/2) ≈ 192.5 min). Heterogeneous rate constants of gaseous ozone reacting with a sorbed fungicide, k(O(3)) (M(-1)·min(-1)), were calculated for both surfaces and indicate losses proceed ∼ 15-fold slower on grapes. The kinetics and mechanism of fungicide removal, supported by gas chromatography- and liquid chromatography-mass spectrometry product analyses, is discussed in the context of facilitating compliance with maximum residue level (MRL) tolerances for fresh produce.