直接进样-液相色谱/串联质谱法(LC-MS)测定水中的酚类化合物

Determination of Phenolic Compounds in Water by Direct Injection-liquid Chromatography/Tandem Mass Spectrometry

采用液相色谱/串联质谱法测定了水中的4种硝基酚类化合物,对流动相、流速、柱温及进样量等条件进行了优化。结果表明,流动相为甲醇和甲酸-甲酸铵溶液（p H=4）,流速0.2 m L/min,色谱柱柱温30℃,进样量10μL,硝基酚类化合物含量在0.5~50μg/L时,校准曲线呈较好的线性关系,相关系数均大于0.999,最低检出限为0.044~0.107μg/L,加标回收率为81.8%~103%,相对标准偏差为1.6%~8.4%。该方法重现性好、灵敏度高、操作简便,有一定的实际应用价值。

A liquid chromatography/tandem mass spectrometric method was used for the determination of 4 kinds of nitro phenolic compounds in water. Experimental conditions such as flow rate,column temperature and injection volume were optimized. The results showed that when the mobile phase was methanol and formic acid-ammonium formate aqueous solution（p H=4）, flow rate was 0.2 m L/min, column temperature was 30 ℃ and the injection volume was 10 μL, the concentration of nitro phenolic compounds content were between 0.5 and 50 μg/L, calibration curve showed good linear relationship with the correlation coefficient of r was over 0.999. The limits of detection were between 0.044 and 0.107 μg/L. The recoveries were between 81.8 % and 103 %. The repeatability expressed as relative standard deviation was between 1.6 % and 8.4 %. The method is quick, simple and sensitive, showing potential in practical applications.