采用吡咯烷丁酸键合硅胶固相萃取法，通过气相色谱-质谱法分析污水中的多氯联苯。
Solid phase extraction with pyrenebutyric acid-bonded silica for analysis of polychlorinated biphenyls in sewage water by gas chromatography-mass spectrometry.
机构信息
Institute of Hydrobiology, Chinese Academy of Sciences, Wuhan, China.
出版信息
Chemosphere. 2010 Nov;81(8):1000-5. doi: 10.1016/j.chemosphere.2010.09.016. Epub 2010 Sep 29.
A solid phase extraction (SPE) method using pyrenebutyric acid-bonded silica (PYB) as sorbent was developed to determine 23 polychlorinated biphenyls (PCBs) in sewage water by gas chromatography-mass spectrometry (GC-MS). Factors were optimized in SPE procedures including elution solvent, pH, and cartridge burden. The recoveries of 23 PCB congeners were 69.44-111.91% under optimized conditions. Comparisons were also conducted among PYB-SPE, C(18)-SPE and United States Environmental Protection Agency 608 (USEPA608) methods in the analysis of PCBs in sewage water samples. The results showed that the performance of PYB-SPE method was similar with USEPA608 method and better than C(18)-SPE method. Both PYB-SPE and USEPA608 methods were then employed to analyze PCBs in real spiked sewage water samples. The recoveries of PCB congeners determined by PYB-SPE method ranged from 70.6% to 92.4% in real spiked sewage water samples which were identified to be in accordance with USEPA608 method. Limits of detection (LOD) were in the range of 0.06-0.22ngL(-1) for PCB congeners. The optimized PYB-SPE method was successfully applied to the determination of PCBs in sewage water samples.
采用吡咯烷丁酸键合硅胶（PYB）作为吸附剂的固相萃取（SPE）方法，通过气相色谱-质谱（GC-MS）法测定污水中的 23 种多氯联苯（PCBs）。优化了 SPE 程序中的洗脱溶剂、pH 值和萃取柱负荷等因素。在优化条件下，23 种 PCB 同系物的回收率为 69.44-111.91%。还比较了 PYB-SPE、C（18）-SPE 和美国环保署 608 法（USEPA608）在污水中 PCB 分析中的性能。结果表明，PYB-SPE 法的性能与 USEPA608 法相似，优于 C（18）-SPE 法。然后，PYB-SPE 和 USEPA608 方法都被用于分析实际加标污水中的 PCB。通过 PYB-SPE 法测定的 PCB 同系物的回收率在实际加标污水样品中为 70.6%-92.4%，与 USEPA608 法一致。PCB 同系物的检出限（LOD）范围为 0.06-0.22ngL（-1）。优化的 PYB-SPE 方法成功应用于污水中 PCB 的测定。
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