^(19)F-NMR定量检测1-氰基-2,2,2-三氟-1-乙酸苯乙酯的参数优化

Parameter optimization for ^(19)F-NMR quantitative detection of 1-cyano-2,2,2-trifluoro-1-phenylethylacetate

建立了核磁共振氟谱法测定氰化物的氟化衍生化合物1-氰基-2,2,2-三氟-1-苯乙基乙酸酯(CTPA)含量的方法。以乙酸3-氟苄酯为内标,采用5mm Auto XBB探头,探头温度298.2K,考察了不同浓度化合物的定量条件;通过比较化合物样品定量峰与内标物质响应峰面积,计算化合物的含量。结果该化合物的19 F-NMR检测方法在0.5~50μg/mL具有良好的线性(r2=0.9966),该方法的定量限0.5μg/mL,检出限0.2μg/mL;同时考察了该化合物在不同浓度下的测量准确度。

This paper established a method for determination of 1-cyano-2,2,2-trifluoro-l-phenylethyl- acetate compound which was fluorinated derivative cyanide. Using acetic acid 3-fluoro-phenyl ester as the internal standard, the 5mm Auto XBB probe was adopted and the probe temperature was 298.5K. The quantitative conditions of the compounds in different concentrations were investigated. The compound content was calculated by comparing the peak area of the compound with the peak area of the internal standard substance. The result showed that the ^19F-NMR detection method had a good linearity （r^2= 0. 9966） in the range of 0.5- 50μg/mL and the limit of quantification was 0.5μg/mL, the limit of detection was 0.2μg/mL. At same time the accuracy at different concentrations were also investigated.