GC-MS Determination of Di-(2-ethylhexyl)-phthalate in Water with Micro-solvent Extraction
摘 要
取水样25 mL,加入无水硫酸钠3.0 g,加入环己烷2.0 mL,振荡萃取3 min。移取萃取了邻苯二甲酸二(2-乙基己基)酯(DEHP)的上层有机相2.0 μL注入HP-5毛细管柱(30 m×0.32 mm,0.25 μm)色谱分离后进行质谱测定。DEHP的质量浓度在50.0 μg·L-1以内与其峰面积呈线性关系,方法的检出限(3S/N)为0.052 μg·L-1。分析了早、中、晚不同时间的天津市自来水,并用标准加入法做回收试验,测得回收率在97.0%~109.4%之间,测定值的相对标准偏差(n=6)均小于2.5%。
Abstract
3.0g of anhydrous Na2SO4 was added to 25 mL of the water sample, which was then extracted by shaking for 3 min with 2.0 mL of cyclohexane. 2.0 μL of the supernatant organic phase containing di-(2-ethylhexyl)-phthalate (DEHP), was introduced into the HP-5 (30 m×0.32 mm, 0.25 μm) capillary chromatographic column, separated and determined by MS. Linear relationship between values of peak area and mass concentration of DEHP was obtained in the range within 50.0 μg·L-1, with detection limit (3S/N) of 0.052 μg·L-1. Three samples of the tap water collected in the morning, noon and night, were analysed by this method, and recovery was tested by standard addition method, giving values of recovery in the range of 97.0%-109.4%, with RSD′s (n=6) less than 2.5%.
中图分类号 O657.7
所属栏目 工作简报
基金项目 国家海洋局业务化项目(批准号:1511112000005);中央级公益性科研院所基本科研业务费专项资金项目(K-JBY-WF-2009-T203)
收稿日期 2011/2/26
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备注刘静(1983-),女,天津人,硕士,工程师,主要从事色谱分析方面的研究。
引用该论文: LIU Jing,ZENG Xing-yu,YAN Wei,WANG Yi,LIU Xiao-qi,ZHAO Xu-long. GC-MS Determination of Di-(2-ethylhexyl)-phthalate in Water with Micro-solvent Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2012, 48(5): 597~598
刘静,曾兴宇,烟卫,王意,刘小骐,赵戌龙. 微溶剂萃取-气相色谱-质谱法测定水中邻苯二甲酸二(2-乙基己基)酯[J]. 理化检验-化学分册, 2012, 48(5): 597~598
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【2】陈会明,王超,王星.毛细管气相色谱法测定化妆品中的酞酸酯[J].色谱, 2004,22(3):224.
【3】GABRIELA P, KATERINA H, JAN P, et al. Development of a solid-phase micro-extraction method for the determination of phthalic acid esters in water[J]. Anal Chim Acta, 2002,457:211-223.
【4】戴树桂,张东海,张仁江,等.固相萃取技术预富集环境水样中邻苯二甲酸酯[J].环境科学, 2000(2):66-69.
【5】US EPAMethods for organic chemical analysis of municipal and industrial wastewater. Method 606-phthalate ester[S].
【6】廖艳,余煜棉,赖子尼,等.固相萃取-气相色谱法检测水中的邻苯二甲酸酯[J].化工环保, 2006,26(3):235-238.
【7】邓琳,陈鹏宇,涂建峰,等.固相微萃取-高效液相色谱法测定水中的酞酸二(2-乙基己基)酯[J].分析科学学报, 2005,21(1):27-29.
【8】周益奇,王子健.污水中6种邻苯二甲酸酯的测定[J].分析测试学报, 2009,28(12):1419-1423.
【9】李敏霞,吴京洪,曾玮,等.液相微萃取-气相色谱法测定水样中邻苯二甲酸酯[J].分析化学, 2006,34(8):1172-1174.
【10】张冬梅,陈忠林,沈吉敏,等.液液微萃取气相色谱测定水中邻苯二甲酸二-2-乙基己基酯[J].中国给水排水, 2009,25(12):83-86.
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