Stir bar sorptive extraction with in situ derivatization and thermal desorption–gas chromatography–mass spectrometry for determination of chlorophenols in water and body fluid samples
Stir bar sorptive extraction with in situ derivatization and thermal desorption–gas chromatography–mass spectrometry for determination of chlorophenols in water and body fluid samples
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DOI：
10.1016/j.aca.2004.10.080
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发表时间：
2005-03
影响因子：
6.2
通讯作者：
Migaku Kawaguchi;Y. Ishii;N. Sakui;N. Okanouchi;R. Ito;Koichi Saito;H. Nakazawa
中科院分区：
文献类型：
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作者：
Migaku Kawaguchi;Y. Ishii;N. Sakui;N. Okanouchi;R. Ito;Koichi Saito;H. Nakazawa
建立了测定自来水、河水和人尿样中2，4-二氯苯酚(2，4-DCP)、2，4，6-三氯苯酚(2，4，6-TrCP)、2，3，4，6-四氯苯酚(2，3，4，6-TECP)和五氯苯酚(PCP)的现场衍生热解吸气相色谱-质谱法(GC-MS)。考察了乙酸酐衍生化条件和萃取时间等SBSE条件。测定自来水、河水和人体尿样中氯酚的检出限分别为1~2、1~2和10~20pgml−1(Ppt)。氯代酚的校正曲线线性良好，相关系数大于0.99。加入2，4-二氯苯酚-d5、2，4，6-三氯苯酚-13C6、2，3，4，6-四氯苯酚-13C6和五氯苯酚-13C6的加标校正后，样品中氯酚的平均回收率均大于95%。该方法简便、准确、灵敏、选择性好，可用于液体样品中痕量氯酚的测定。
A new method, stir bar sorptive extraction (SBSE) with in situ derivatization and thermal desorption (TD)–gas chromatography–mass spectrometry (GC–MS), which is used for the determination of trace amounts of chlorophenols, such as 2,4-dichlorophenol (2,4-DCP), 2,4,6-trichlorophenol (2,4,6-TrCP), 2,3,4,6-tetrachlorophenol (2,3,4,6-TeCP) and pentachlorophenol (PCP), in tap water, river water and human urine samples, is described. The derivatization conditions with acetic acid anhydride and the SBSE conditions such as extraction time are investigated. Then, the stir bar is subjected to TD followed by GC–MS. The detection limits of the chlorophenols in tap water, river water and human urine samples are 1–2, 1–2, and 10–20pgml−1(ppt), respectively. The calibration curves for the chlorophenols are linear and have correlation coefficients higher than 0.99. The average recoveries of the chlorophenols in all the samples are higher than 95% (R.S.D.<10%) with correction using added surrogate standards, 2,4-dichlorophenol-d5, 2,4,6-trichlorophenol-13C6, 2,3,4,6-tetrachlorophenol-13C6and pentachlorophenol-13C6. This simple, accurate, sensitive and selective analytical method may be applicable to the determination of trace amounts of chlorophenols in liquid samples.