Rapid analytical methods to measure pentachlorophenol in wood
Rapid analytical methods to measure pentachlorophenol in wood
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DOI：
10.1021/jf9605963
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发表时间：
1997-04-01
影响因子：
6.1
通讯作者：
Turesky, RJ
中科院分区：
文献类型：
--
作者：
Gremaud, E;Turesky, RJ
用甲醇：0.1%乙酸提取木材中的五氯苯酚（PCP）。在含有甲苯和0.1 M Na 2CO 3（pH 11.4）的两相溶剂中，用乙酸酐对提取物进行衍生化，并使用[C-13（6）]PCP作为内标物，通过气相色谱-质谱法（GC-MS）对乙酸五氯苯酯进行定量。第二种检测方法是在硝酸介导下将五氯苯酚氧化为四氯-1，4-苯醌后采用薄层色谱法。第三种方法是比色法，需要在酸性和碱性pH值下对五氯苯酚和甲苯进行液-液分配。然后，PCP在过硫酸钠存在下与4-氨基安替比林偶联，形成染料，在580 nm处测量。当使用100 mg木材进行分析时，GC-MS的检测限接近50 ppb，TLC的检测限接近1 ppm，当使用1 g木材进行检测时，比色法的检测限接近1 ppm。所有三种方法得出的五氯苯酚估计值具有可比性。
Pentachlorophenol (PCP) was measured in wood following extraction with methanol:0.1% acetic acid. The extract was derivatized with acetic anhydride in a biphasic solvent containing toluene and 0.1 M Na2CO3 (pH 11.4), and pentachlorophenyl acetate was quantitated by gas chromatography-mass spectrometry (GC-MS) using [C-13(6)]PCP as an internal standard. A second detection method employed thin layer chromatography (TLC) after nitric acid-mediated oxidation of PCP to tetrachloro-1,4-benzoquinone. The third method was by colorimetry and required a liquid-liquid partitioning of PCP under acidic and alkaline pH against toluene. Then, PCP was coupled to 4-aminoantipyrine in the presence of sodium persulfate to form a dye which was measured at 580 nm. The limit of detection approached 50 ppb by GC-MS and 1 ppm by TLC when 100 mg of wood was used for analysis and 1 ppm for the colorimetric method when 1 g of wood was used for detection. The estimates of PCP were comparable for all three methods.