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微孔竹炭固相萃取与高效液相色谱-电喷雾串联质谱联用测定环境水中痕量三氯生。

Determination of trace triclosan in environmental water by microporous bamboo-activated charcoal solid-phase extraction combined with HPLC-ESI-MS.

机构信息

School of Light Chemistry and Environmental Engineering, Shandong Polytechnic University, Jinan, China.

出版信息

J Sep Sci. 2012 Oct;35(20):2781-6. doi: 10.1002/jssc.201200328. Epub 2012 Sep 5.

Abstract

A sensitive and efficient analytical method for triclosan (TCS) determination in water, which involves enrichment with bamboo-activated charcoal and detection with HPLC-ESI-MS, was developed. The influence of several operational parameters, including the eluant and its volume, the flow rate, the volume andacidity of the sample, and the amount of bamboo-activated charcoal, were investigated and optimized. Under the optimum conditions, linearity of the method was observed in the range of 0.02-20 μg/L, with correlation coefficients (r(2) ) >0.9990. The limit of detection was 0.002 μg/L based on the ratio of chromatographic signal to baseline noise (S/N = 3). The spiked recoveries of TCS in real water samples were achieved in the range of 97.6-112.5%. The proposed method was applied to analyze TCS in real aqueous samples. All the surface water samples collected in Xiaoqing River had detectable levels of TCS with concentrations of 42-197 ng/L.

摘要

建立了一种灵敏、高效的水样中三氯生(TCS)分析方法,该方法采用竹炭吸附富集,高效液相色谱-电喷雾串联质谱法(HPLC-ESI-MS)检测。考察并优化了几种操作参数的影响,包括洗脱剂及其体积、流速、样品体积和酸度以及竹炭的用量。在最佳条件下,该方法在 0.02-20 μg/L 范围内呈良好的线性关系,相关系数(r(2))>0.9990。基于色谱信号与基线噪声的比值(S/N = 3),检测限为 0.002 μg/L。TCS 在实际水样中的加标回收率在 97.6-112.5%范围内。该方法用于分析实际水样中的 TCS。从小清河采集的所有地表水样品均检测到 TCS,浓度为 42-197 ng/L。

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