反相高效液相色谱法测定合成产物2-硝基芴酮的含量

建立了一种反相高效液相色谱法测定2-硝基芴酮含量的方法。液相色谱条件为:EliteHypersil ODS2C18色谱柱(4.6mm×250mmi.d.,5μm),甲醇-四氢呋喃-水为流动相(体积比为65∶15∶35)。在流速1.0mL/min,检测波长254nm,柱温25℃条件下,产物2-硝基芴酮与原料芴酮、副产物2,7-二硝基芴酮在2-硝基芴酮浓度为5—30mg/L范围内分离效果良好,峰面积与质量浓度呈良好的线性关系,相关系数为0.9985;平均回收率值大于99.00%,相对标准偏差小于1.00%。结果表明,该方法具有操作简便、精密度和准确性高的特点,可适用于工业生产2-硝基芴酮含量的测定。

Determination of 2-Nitrofluorenone in Synthetic Products by High Performance Liquid Chromatography

2-Nitrofluorenone was determined by high performance liquid chromatography（HPLC） with the chromatographic conditions of Elite Hypersil ODS2 C18 column（4.6×250mm）; the mobile phase of methanol-THF-water（65：15：35 V/V）; the flow rate of 1.0mL/min;the detection wavelength of 254nm,and the column temperature of 25℃.The product 2-nitrofluorenone was well separated from starting material fluorenone and by-product 2,7-nitrofluorenone when the concentration of 2-nitrofluorenone was 5—30mg/L,and its peak area had a good linear relationship with its content（r=0.9985）; the average recovery was higher than 99.00% and the RSD was lower than 1.00%.This method is rapid and reliable,and can be applied for the determination of the industrial preparation of 2-nitrofluorenone.