Saraji Mohammad, Ghambari Hoda
Department of Chemistry, Isfahan University of Technology, Isfahan, Iran.
J Sep Sci. 2015 Oct;38(20):3552-9. doi: 10.1002/jssc.201500556. Epub 2015 Sep 9.
Trace analysis of chlorophenols in water was performed by simultaneous silylation and dispersive liquid-liquid microextraction followed by gas chromatography with mass spectrometry. Dispersive liquid-liquid microextraction was carried out using an organic solvent lighter than water (n-hexane). The effect of different silylating reagents on the method efficiency was investigated. The influence of derivatization reagent volume, presence of catalyst and derivatization/extraction time on the yield of the derivatization reaction was studied. Different parameters affecting extraction efficiency such as kind and volume of extraction and disperser solvents, pH of the sample and addition of salt were also investigated and optimized. Under the optimum conditions, the calibration graphs were linear in the range of 0.05-100 ng/mL and the limit of detection was 0.01 ng/mL. The enrichment factors were 242, 351, and 363 for 4-chlorophenol, 2,4-dichlorophenol, and 2,4,6-trichlorophenol, respectively. The values of intra- and inter-day relative standard deviations were in the range of 3.0-6.4 and 6.1-9.9%, respectively. The applicability of the method was investigated by analyzing water and wastewater samples.
采用同时硅烷化和分散液液微萃取结合气相色谱-质谱联用技术对水中的氯酚进行痕量分析。分散液液微萃取使用比水轻的有机溶剂（正己烷）进行。研究了不同硅烷化试剂对方法效率的影响。考察了衍生化试剂体积、催化剂的存在以及衍生化/萃取时间对衍生化反应产率的影响。还研究并优化了影响萃取效率的不同参数，如萃取剂和分散剂溶剂的种类和体积、样品的pH值以及盐的添加量。在最佳条件下，校准曲线在0.05 - 100 ng/mL范围内呈线性，检测限为0.01 ng/mL。4-氯酚、2,4-二氯酚和2,4,6-三氯酚的富集因子分别为242、351和363。日内和日间相对标准偏差值分别在3.0 - 6.4%和6.1 - 9.9%范围内。通过分析水和废水样品考察了该方法的适用性。
