食品科学 ›› 2011, Vol. 32 ›› Issue (18): 164-167.doi: 10.7506/spkx1002-6630-201118034

• 分析检测 • 上一篇    下一篇

固相萃取检测养殖水体中邻苯二甲酸酯残留

马保华1,王兆梅2,*,李 娜2,胡冬生1,李 贺1,吕振华3   

  1. 1. 南海出入境检验检疫局
    2.华南理工大学轻工与食品学院 3.惠州出入境检验检疫局
  • 出版日期:2011-09-25 发布日期:2011-09-24
  • 基金资助:
    国家自然科学基金面上基金项目(B5100800);广东检验检疫局科技计划项目(2006GDK13); 广东省大学生创新实验项目(S1010561061)

Determination of Phthalic Acid Ester Residues in Aquaculture Water by Solid Phase Extraction Coupled to Gas Chromatography

MA Bao-hua1,WANG Zhao-mei2,*,LI Na2,HU Dong-sheng1,LI He1,LU Zhen-hua3   

  1. (1. Nanhai Entry-Exit Inspection and Quarantine Bureau, Foshan 528200, China; 2. College of Light Industry and Food Science, South China University of Technology, Guangzhou 510640, China; 3. Huizhou Entry-Exit Inspection and Quarantine Bureau, Huizhou 516001, China)
  • Online:2011-09-25 Published:2011-09-24

摘要: 建立固相萃取-气相色谱检测水体中6种邻苯二甲酸酯类物质的方法。采用正交设计确定最佳固相萃取条件为洗脱剂正己烷-丙酮(30:1,V/V)、洗脱体积6mL、洗脱速率2mL/min、上样速率8mL/min,采用氢火焰离子化检测器的气相毛细管色谱。结果表明:邻苯二甲酸酯的检测限为1.4~3.6μg/L,线性范围在1~80mg/L之间,相关系数为0.995以上;低、高质量浓度加标回收率在72%~100%之间,相对标准偏差均小于10%。采用此方法对广东省12个水产养殖基地的养殖水进行邻苯二甲酸酯类物质测定,发现所有检测水样中均有邻苯二甲酸酯类物质残留(4.2~171.5μg/L),其污染程度与地域密切相关。

关键词: 固相萃取, 邻苯二甲酸酯, 养殖水体

Abstract: A method for the simultaneous determination of 6 phthalic scid esters (PAEs) aquaculture in water by solid phase extraction (SPE) and gas chromatography detection was developed. The SPE conditions were optimized using orthogonal array design as follows: n-hexane-acetone (30:1, V/V) as elution solvent at a flow rate of 2.0 mL/min, elution volume 6 mL, and sample loading rate 6.0 mL/min. Enriched samples were determined using a capillary gas chromatograph with flame ionization detector. The ldetection limits of 6 PAEs were in the range of 1.4-3.6μg/L. The method displayed a good linearity over the range of 1 to 80 mg/L, with a correlation coefficient of larger than 0.995. The recoveries of the 6 PAEs across low, medium high spike levels were 72%-117% and the relative standard deviations all lower than 10%. The PAEs in 12 samples from typical aquatic breeding areas in Guangdong province were detected by the established method. All samples were found to be polluted by total PAEs concentration in the range of 4.2-171.5 μg/L. Moreover, the contaminations of PAEs were closely associated with geographic areas.

Key words: phthalic acid esters, aquaculture water, solid phase extraction

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