高效液相色谱法测定水中苦味酸

摘要

Picric acid in water is directly measured with high performance liquid chromatography-UV detector. The clean water samples were directly detected after filtered by 0.22μm PTFE. The complex water samples were determined after extraction and purification. The chromatographic column was the Symmetry C18 and the methanol (0.1% formic acid):water (0.1% formic acid) is the mobile phase, the column temperature is 40℃ and the measurement wavelength is 357 nm. Under the conditions, picric acid has excellent peak shape, retention time and calibration curve and the correlation coefficient is 0.9999. With the method, the detection limit is 0.02 mg/L, the quantification limit is 0.08 mg/L, the relative standard deviation is 1.2% to 2.1%, and the recovery rate of standard addition is 95.4% to 101%. With simple and quick operation and high sensitivity, the method can separate the picric acid from other phenolic distractors effectively.%采用高效液相色谱法直接测定水中的苦味酸.干净的水样经0.22μm聚四氟乙烯亲水滤头过滤后直接进样,成分复杂的水样则经液液萃取净化,取萃取后水相进样.采用Symmetry C18色谱柱,流动相为甲醇(0.1%甲酸):水(0.1%甲酸)、柱温40℃、检测波长357 nm,为最佳的检测条件.在该检测条件下,苦味酸有较好的峰形和保留时间,绘制的校准曲线线性良好,相关系数为0.9999.方法检出限为0.02 mg/L,定量限为0.08 mg/L,相对标准偏差在1.2%~2.1%之间,加标回收率为95.4%~101%.该方法操作简便快速、灵敏度高,能有效将苦味酸与其他酚类干扰物分离.