超声提取-气相色谱/串联质谱法测定水厂污泥中五氯酚

Determination of Trace Pentachlorophenol in Sludge from Water Treatment Plants by Ultrasonic Extraction/Derivatization Gas Chromatography/Tandem Mass Spectrometry

建立了一种测定水厂污泥中痕量五氯酚的超声提取-衍生化气相色谱/串联质谱分析方法。水厂污泥经酸化处理后,以正己烷/丙酮(1∶1)为提取溶剂,超声提取其中的痕量五氯酚。提取物用碳酸钾纯化、乙酸酐衍生化后进行气相色谱/串联质谱分析。该方法线性范围为0.20～31.00 ng/mL,线性相关系数为0.999 6,定量下限为0.10μg/kg(S/N=10),加标回收率为87.25%～111.13%,相对标准偏差为6.13%～9.27%。

An ultrasonic extraction/derivatization gas chromatography/tandem mass spectrometry method was established to determine the content of trace pentachlorophenol in sludge from water treatment plants. The sludge was first acidified, then was uhrasonically extracted with henxane/acetone （1 ： 1 ） as the extraction solvent. The extract was purified by K2CO3 and then derived with acetic anhydride. The derivative product was analyzed by gas chromatography/tandem mass spectrometry. The linear range was 0.20 to 31.00 ng/mL with a linear correlation coefficient of 0. 999 6. The lower limit of quantification was 0.10 μg/kg （S/N = 10）. The spiked recovery varied from 87.25% to 111.13% while the relative standard deviation changed from 6.13% to 9.27%.