分散液相微萃取-气相色谱法测定水中的苯乙酮及其衍生物.docVIP

分散液相微萃取-气相色谱联用法测定水样中的苯乙酮及其衍生物 叶存玲，王和平，刘清玲，王治科 （河南师范大学化学化工学院，河南省环境污染控制重点实验室，黄淮水环境与污染防治省部共建教育部重点实验室，河南 新乡 453007） 摘要：建立了分散液相微萃取-气相色谱联用方法测定水中5种苯乙酮类化合物残留的新方法。采用氯仿为萃取剂，乙腈为分散剂，考察了萃取剂和分散剂的种类及体积，溶液pH值及盐析效果等因素对萃取效果的影响。在优化实验条件下，该方法对苯乙酮、2-羟基苯乙酮、对溴苯乙酮、对甲氧基苯乙酮和二苯乙酮的线性范围分别为0.5-100.0 μg L-1、0.9-100 μg L-1、1.0-100.0 μg L-1、0.7-100.0 μg L-1和0.8-100.0 μg L-1。检出限和6次重复测定的相对标准偏差分别为0.3-0.6 μg L-1和2.5%~8.5%。该方法应用于自来水、地下水、泉水和湖水样品的分析测定，回收率在90.2%-113.9%之间。 关键词：分散液相微萃取；气相色谱法；苯乙酮及其衍生物；水样 Determination of hypnone derivatives in water samples by dispersive liquid-liquid microextraction-gas chromatography YE Cun-ling*, WANG He-ping, LIU Qing-ling, WANG Zhi-ke (School of Chemistry and Chemical Engineering, Henan Key Laboratory for Environmental Pollution Control, Key Laboratory for Yellow River and Huai River Water Environment and Pollution Control, Ministry of Education, Henan Normal University, Xinxiang Henan 453007) Abstract: A simple and efficient method known as dispersive liquid-liquid microextraction was demonstrated for the extraction of hypnone derivatives in real water samples prior to GC-FID. Several related parameters, including volumes and types of extraction reagent and dispersive reagent, pH and salinity of solution, that could affect the extraction efficiencies were also investigated and optimized. Under the optimum conditions, a linear range was obtained in the range of 0.5-100.0 μg L-1 for hypnone, 0.9-100.0 μg L-1 for 2-hydroxy acetophenone 1.0-100.0 μg L-1 for p-bromoacetophenone, 0.73-100 μg L-1 for p-acetylanisole and 0.77-100 μg L-1 for diphenyl ketone, respectively. The limits of detection (LODs) (S/N=3) values were in the range of 0.3-0.6 μg L-1. The relative standard deviations of five hypnone derivatives for six repeated determinations were in the range of 2.5%- 8.5%. The relative recoveries of the five analytes in tap, well, lake and fountain water samples were in the range of 90.2-113.9%. Keywords: Dispersive liquid-liquid microextraction; Gas chromatography; Hyp