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顶空进样-固相微萃取测定饮用水源水中吡啶

赖永忠

赖永忠. 顶空进样-固相微萃取测定饮用水源水中吡啶[J]. 岩矿测试, 2011, 30(5): 596-600.
引用本文: 赖永忠. 顶空进样-固相微萃取测定饮用水源水中吡啶[J]. 岩矿测试, 2011, 30(5): 596-600.
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LAI Yong-zhong. Determination of Pyridine in Drinking Source Water by Head Space Sampling-Solid Phase Microextraction[J]. Rock and Mineral Analysis, 2011, 30(5): 596-600.
Citation: LAI Yong-zhong. Determination of Pyridine in Drinking Source Water by Head Space Sampling-Solid Phase Microextraction[J]. Rock and Mineral Analysis, 2011, 30(5): 596-600.
shu

顶空进样-固相微萃取测定饮用水源水中吡啶

  • 汕头市环境保护监测站, 广东 汕头 515041

Determination of Pyridine in Drinking Source Water by Head Space Sampling-Solid Phase Microextraction

  • Shantou Enviromental Monitoring Station, Shantou 515041, China

摘要

    摘要
  • 摘要: 用75 μm CarboxenTM-Polydimethylsiloxane(CAR-PDMS)固相微萃取头顶空萃取15 mL水样中的吡啶,萃取物用气相色谱-质谱法进行分离和检测,采用内标法和质谱的选择离子监测模式进行定量分析。优化了顶空进样-固相微萃取条件,获得较佳的萃取温度(58.0℃)和萃取时间(40 min)。在优化的条件下,方法检出限为1.5 μg/L,标准曲线的线性相关系数为0.9994,线性范围为2.5~50.0 μg/L;饮用水源水和纯水加标平均回收率为75.6%~81.3%,相对标准偏差(RSD,n=6)为9.60%~12.21%。使用顶空萃取方式可避免样品基体的复杂性,有利于保护萃取头涂层,同时无需使用有机萃取溶剂;使用质谱检测器可减小假阳性带来的影响。顶空进样-固相微萃取操作简单、环保、灵敏度高,适合用于饮用水源水中吡啶的监测分析。
    Abstract: Pyridine in 15 mL aqueous sample was micro-extracted by using a head space sampling-solid phase microextration system of 75 μm CarboxenTM-Polydimethylsiloxane (CAR-PDMS) fiber. The extractants were measured by Gas Chromatography-Mass Spectrometry (GC-MS) with selected ion monitoring (SIM) mode and internal standard quantitative method. Under the optimum conditions of an extraction temperature of 58.0℃ for 40 min, detection limit, correlation coefficient and linear range were 1.5 μg/L, 0.9994 and 2.5-50.0 μg/L, respectively. The obtained average values of recovery were 75.6%-81.3% (n=6) and the relative standard deviation was 9.60%-12.61% for drinking water samples and pure water with interior spike. Head space sampling-solid phase microextraction (HS-SPME), an organic solvent-free pre-processing method for water sample, can protect SPME coatings, especially for dirty samples. An MS detector has advantages in qualitative analysis and avoids the fake positive signal effect. Head space-solid phase microextraction is a convenient and sensitive method, which is capable of analyzing pyridine in drinking water.
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出版历程
  • 收稿日期:  2011-03-04
  • 修回日期:  2011-05-12

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