Solid phase analytical derivatization of anthropogenic and natural phenolic estrogen mimics with pentafluoropyridine for gas chromatography-mass spectrometry.
Solid phase analytical derivatization of anthropogenic and natural phenolic estrogen mimics with pentafluoropyridine for gas chromatography-mass spectrometry.
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DOI：
10.1016/j.chroma.2011.10.060
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发表时间：
2011-12
期刊：
影响因子：
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通讯作者：
Sanka N. Atapattu;J. Rosenfeld
中科院分区：
文献类型：
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作者：
Sanka N. Atapattu;J. Rosenfeld
以五氟吡啶为衍生化试剂，建立了测定4种内分泌干扰物4-叔丁基苯酚、4-叔辛基苯酚、双酚A和17-β-雌二醇的简便、低成本、快速、灵敏的方法。在没有任何相转移催化剂(PTC)或离子对机制的情况下，通过固相分析衍生化(SPAD)技术同时萃取和衍生化测定了这些EDCs。水中4-叔丁基苯酚和17-β-雌二醇的回收率分别为71%和106%；尿样中17-β-雌二醇和腐植酸溶液中的回收率分别为61%和91%；腐植酸溶液中17-β-雌二醇和4-叔辛基酚的回收率分别为59%和104%。以男性尿液为基质，在1-40 ng/m L范围内构建校正曲线，相关系数大于0.99。4-叔丁基苯酚、双酚A和17β-雌二醇的最低定量限为5 ng/mL，4-叔辛基酚的最低定量限为1 ng/mL。将该方法应用于EDCs的测定，检测到的4-叔辛基苯酚、双酚A和17-β-雌二醇的浓度与文献中的浓度相当。该方法具有分析速度快、试剂用量少、衍生化专属性强等优点。
A simple, low cost, fast and sensitive method is reported for the determination of the four endocrine disrupting chemicals (EDCs) 4-tert-butylphenol, 4-tert-octylphenol, bisphenol A and 17β-estradiol using pentafluoropyridine as the derivatizing reagent. These EDCs were determined by simultaneous extraction and derivatization in a solid phase analytical derivatization (SPAD) technique without the aid of any phase transfer catalyst (PTC) or an ion-pair mechanism. Recoveries of analytes as their tetrafluoropyridyl derivatives from water ranged from 71% for 4-tert-butylphenol to 106% for 17β-estradiol; from urine they ranged from 61% for 17β-estradiol to 91% for 4-tert-octylphenol; and from humic acids solution the ranged from 59% for 17β-estradiol to 104% for 4-tert-octylphenol in humic acid solutions. Calibration curves were constructed from a matrix of human male urine in the range 1–40ng/mL and had coefficients of correlation greater than 0.99. For 4-tert-butylphenol, bisphenol A and 17β-estradiol the limits of quantitation were 5ng/mL and for 4-tert-octylphenol it was 1ng/mL. This method was applied to determine EDCs and detected 4-tert-octylphenol, bisphenol A and 17β-estradiol in concentrations comparable to those found in the literature. The method offers advantages in speed of analysis, reduced reagent and specificity of derivatization.