Determination of phenols in environmental waters using liquid chromatography with electrochemical detection
Determination of phenols in environmental waters using liquid chromatography with electrochemical detection
复制标题
采用电化学检测液相色谱法测定环境水中的酚类物质
DOI：
10.1016/0021-9673(95)01192-7
复制
发表时间：
1996
影响因子：
4.1
通讯作者：
P. Jackson
中科院分区：
文献类型：
--
作者：
B. Paterson;C. Cowie;P. Jackson
讨论了测定环境水中低微克/升浓度的优先污染物酚类的液相色谱方法的发展。使用 Nova-Pak Phenyl 柱进行分离，从 20 mM 乙酸铵（19% 乙腈）到 20 mM 乙酸铵（54% 乙腈）进行凹梯度洗脱，历时 12 分钟，随后使用配备玻碳工作电极的电化学检测器（在 +1150 mV 电位下操作）进行检测。这种方法使样品干扰最小化，实际定量限在低 μg/l 范围内。 LC-ED 方法比现有的 GC 和 GC-MS 苯酚方法具有明显的优势，因为不需要提取样品，因此避免了基于 GC 分析所需的提取、浓缩和溶剂交换步骤中发生的损失。该方法通过参与循环测试计划进行评估，其中包括环境水基质中 11 种优先污染物酚的测定。使用 LC-ED 方法获得的结果和回收率与总体一致结果相比较，十一种酚的回收率范围为 75% 至 118%。实验室间的重现性数据表明了高水平的集体熟练程度，对于加标的炼油厂废水、造纸厂废水和试剂水样品，11 种分析物的总体平均变异系数分别为 18%、18% 和 13%。
The development of a liquid chromatographic method for the determination of priority pollutant phenols at low μg/l levels in environmental waters is discussed. The phenols were separated using a Nova-Pak Phenyl column with concave gradient elution from 20 mM ammonium acetate (19% acetonitrile) to 20 mM ammonium acetate (54% acetonitrile) over 12 min, and subsequently detected using an electrochemical detector equipped with a glassy carbon working electrode, operated at a potential of +1150 mV. This approach resulted in minimal sample interferences and practical quantitation limits in the low μg/l range. The LC-ED method offers a distinct advantage over the established GC and GC-MS phenol methods in that no sample extraction is required, hence avoiding the losses which occur during the extraction, concentration and solvent exchange steps required for the GC-based analyses. The method was evaluated through participation in a round robin testing program, involving determination of the eleven priority pollutant phenols in environmental water matrices. The results and recoveries obtained using the LC-ED method compared well with the overall consensus results, with recoveries ranging from 75% up to 118% for the eleven phenols. The between-laboratory reproducibility data indicated a high level of collective proficiency, with the overall average coefficients of variation for the eleven analytes being 18%, 18% and 13%, for spiked oil refinery effluent, paper mill effluent and reagent water samples, respectively.