Citation: ZHANG Chun-Yan, LIU Zhi-Wei, GOU Gao-Zhang, YANG Qian-Wen, SHI Hai-Yan, WANG Ming-Hua. Study of Absolute Configuration and Residue Analysis Method for Epoxiconazole Enantiomers[J]. Chinese Journal of Analytical Chemistry, ;2018, 46(11): 1778-1784. doi: 10.11895/j.issn.0253-3820.181351
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A method for separation of epoxiconazole enantiomers was established by reversed-phase high performance liquid chromatography (HPLC) on a Lux Cellulose-1 chiral column. The elution order of the epoxiconazole enantiomers was determined by HPLC coupled with a circular dichroism (CD) detector. The absolute configuration of epoxiconazole enantiomer was determined through comparison of experimental and predicted ECD spectra. Based on this, a simple and reliable method for simultaneous determination of epoxiconazole enantiomers in fruits and vegetables samples was established, and the method was systematically evaluated by the precision, accuracy, sensitivity and matrix effect of sample. When using acetonitrile-water (60:40, V/V) as mobile phase with a flow rate of 0.6 mL/min, the epoxiconazole enantiomers were baseline separated at 30℃ and detection wavelength of 220 nm. The first peak eluted from the Lux Cellulose-1 chiral column was confirmed to be (S,R)-(-)-epoxiconazole and the second peak was (R,S)-(+)-epoxiconazole. Excellent linearity of enantiomers was observed within concentration range of 0.1-10 mg/L, and there was no matrix effect. The results of the standard addition experiment showed that the average recovery of epoxiconazole enantiomers in the six matrices was 80.8%-96.7%, with inter-day precision (Relative standard deviation, RSD) of 1.5%-6.1% and intra-day RSD of 1.1%-6.7%. The limits of quantification (LOQs) for two enantiomers in six matrices were 0.05 mg/kg, whereas the limits of detection (LODs) were 0.10-0.15 ng. The analytical method could meet the requirement of simultaneous determination of epoxiconazole enantiomers in food and environmental sampless
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