Citation: ZHAO Yue-Chen, ZHANG Xin-Zhong, LUO Feng-Jian, ZHOU Li, CHEN Zong-Mao, CUI Xin-Yi. Residue Determination of cis-Epoxiconazole Enantiomers in Fruit and Tea by Ultra Performance Convergence Chromatography Combined with Quadrupole Time-of-Flight Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2016, 44(8): 1200-1208. doi: 10.11895/j.issn.0253-3820.160047 shu

Residue Determination of cis-Epoxiconazole Enantiomers in Fruit and Tea by Ultra Performance Convergence Chromatography Combined with Quadrupole Time-of-Flight Mass Spectrometry

1.
College of Horticulture and Landscape, Tianjin Agricultural University, Tianjin 300384, China;
2.
Research Center of Quality Safety for Agricultural Products, Tea Research Institute, Chinese Academy of Agricultural Sciences, Hangzhou 310008, China

Received Date: 18 January 2016
Revised Date: 4 April 2016

Fund Project: This work was supported by the National Natural Science Foundation of China (No. 21107137)

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A chiral separation and residue determination method for cis-epoxiconazole enantiomers in apple, grape and tea samples was developed and validated by ultra performance convergence chromatography combined with quadrupole time-of-flight mass spectrometry (UPC²-QTOF/MS). The Chrial CCA column was used to separate cis-epoxiconazole enantiomers and the chromatography conditions (mobile phase modifier and proportion, column temperature, automated backpressure regulator, and auxiliary solvent) were optimized. Samples were extracted by acetonitrile, and respectively purified by Cleanert TPT or Pesti-Carb solid phase extraction (SPE) columns, then analyzed by UPC²-QTOF/MS. The optimum conditions were as follows:mobile phase was CO₂/isopropanol(95:5, V/V), flow-rate was 2.0 mL/min, automated backpressure regulator (ABPR) was 13.79 MPa, column temperature was 30℃, with a post-column mauxiliary solvent of methanol/water (1:1, V/V) containing 2 mmol/L ammonium formate. The analyte was quantified by matrix external standard method. The results showed that linear range of this method was 0.01-1.00 mg/L, and the correlation coefficients were above 0.99. The recoveries of cis-epoxiconazole enantiomers at three spiked levels (0.005, 0.025 and 0.25 mg/kg) in fruit matrix were 67.9%-92.8% with relative standard deviations (RSDs, n=6) less than 10%, and the limit of quantification (LOQ) of enantiomers was 0.005 mg/kg. The recoveries of cis-epoxiconazole enantiomers at three spiked levels (0.01, 0.05 and 0.5 mg/kg) in black tea were 74.1%-84.0% with RSDs (n=6) less than 8%, and the LOQ for these two enantiomers was 0.01 mg/kg. This method is rapid, convenient and reliable, and could meet the requirement of residue analysis.
- Chiral enantiomers,
- Residue analysis,
- cis-Epoxiconazole,
- Apple,
- Grape,
- Tea,
- Ultra performance convergence chromatography combined with quadrupole time-of-flight mass spectrometry
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沈阳化工大学材料科学与工程学院沈阳 110142