School of Chemistry and Environment, South China Normal University, Guangzhou 510006, China.
School of Chemistry and Environment, South China Normal University, Guangzhou 510006, China.
Talanta. 2018 Sep 1;187:40-46. doi: 10.1016/j.talanta.2018.04.097. Epub 2018 May 1.
Herein, we developed a rapid supercritical fluid chromatography (SFC) method for chiral separation and enantioselective determination of prothioconazole in soil and tomatoes. The potential effects of chiral stationary phases, co-solvents, column temperature, and back pressure on enantioseparation of prothioconazole have been studied in detail. Two prothioconazole enantiomers were best separated on cellulose tris(3, 5-dimethylphenylcarbamate)-coated chiral stationary phase with CO-2-propanol (80:20, v/v) as the mobile phase, and the run time through SFC (about 4 min) was five-fold shorter than HPLC. Then, through comparing the experimental vibrational circular dichroism spectrum of the later-eluted component with the calculated pattern based on the (R)-configuration, it should be (R)-(-)-prothioconazole. Moreover, the modified QuEChERS (quick, easy, cheap, effective, rugged and safe) extraction and cleanup procedures were applied in enantiomeric analysis of prothioconazole in two matrices. Good linearity (R ≥ 0.9992) and recoveries (91.84-101.66%, RSD ≤ 3.98%) for two enantiomers were achieved. This proposed method showed good accuracy and precision, and might be suitable for fast enantioselective determination and residual quantitative analysis of prothioconazole in food and environmental samples.
本文建立了一种快速超临界流体色谱（SFC）方法，用于对土壤和番茄中丙硫菌唑的对映体拆分和手性选择性测定。详细研究了手性固定相、共溶剂、柱温、背压对丙硫菌唑对映体拆分的影响。两种丙硫菌唑对映体在手性固定相纤维素三（3,5-二甲基苯基氨基甲酸酯）上最佳分离，以 CO2-异丙醇（80:20，v/v）为流动相，SFC 运行时间（约 4 分钟）比 HPLC 缩短了五倍。然后，通过比较后洗脱组分的实验振动圆二色光谱与基于（R）-构型计算的模式，确定它应该是（R）-（-）-丙硫菌唑。此外，改良的 QuEChERS（快速、简单、廉价、有效、耐用和安全）提取和净化程序被应用于两种基质中丙硫菌唑的对映体分析。两种对映体均获得了良好的线性（R≥0.9992）和回收率（91.84-101.66%，RSD≤3.98%）。该方法具有良好的准确性和精密度，可能适用于食品和环境样品中丙硫菌唑的快速对映体选择性测定和残留定量分析。
