Determination of 4-tert.-octylphenol and 4-nonylphenol in laboratory animal feed sample by stir bar sorptive extraction followed by liquid desorption and column-switching liquid chromatography-mass spectrometry with solid-phase extraction.
Determination of 4-tert.-octylphenol and 4-nonylphenol in laboratory animal feed sample by stir bar sorptive extraction followed by liquid desorption and column-switching liquid chromatography-mass spectrometry with solid-phase extraction.
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DOI：
10.1016/j.chroma.2004.06.066
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发表时间：
2004-08
期刊：
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通讯作者：
Migaku Kawaguchi;Shima Takahashi;Fumie Seshimo;N. Sakui;N. Okanouchi;R. Ito;K. Inoue;Y. Yoshimura;S. Izumi;T. Makino;H. Nakazawa
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作者：
Migaku Kawaguchi;Shima Takahashi;Fumie Seshimo;N. Sakui;N. Okanouchi;R. Ito;K. Inoue;Y. Yoshimura;S. Izumi;T. Makino;H. Nakazawa
建立了一种新的测定4-叔丁基-1，4-二氢喹啉的分析方法。实验室动物饲料样品中辛基酚（OP）和4-壬基酚（NP）的测定，包括搅拌棒吸附萃取（SBSE）、液相解吸（LD）和固相萃取（SPE）的柱切换液相色谱-质谱（CS-LC-MS）。该方法需要通过稳定的同位素标记的替代标准品氘4-叔-辛基苯酚（OP-d）和[2 H5] 4-（1-甲基）辛基苯酚（m-OP-d5）。通过超声处理将进料样品与甲醇均质化。离心后，使用涂有聚二甲基硅氧烷的搅拌棒在室温（25°C）下对上清液进行提取120分钟。萃取后，使用乙腈通过LD从搅拌棒解吸分析物。然后，通过具有SPE的CS-LC-MS分析液体样品。添加20 ngg − 1 OP和NP的实验室饲料样品的平均回收率分别为99.5%和103.8%，使用添加的替代标准进行校正。饲料样品中OP和NP的定量限分别为1 ngg-1和5 ngg-1。商业实验室动物饲料样品中OP和NP的测量导致检测到sub ngg− 1 NP
A novel analytical method has been developed for the determination of 4-tert.-octylphenol (OP) and 4-nonylphenol (NP) in laboratory animal feed samples, which involves stir bar sorptive extraction (SBSE) followed by liquid desorption (LD) and column-switching liquid chromatography–mass spectrometry (CS-LC–MS) with solid-phase extraction (SPE). The method required correction by stable isotopically labeled surrogate standards, deuterium 4-tert.-octylphenol (OP-d) and [2H5] 4-(1-methyl)octylphenol (m-OP-d5). A feed sample was homogenized with methanol by ultrasonication. After centrifugation, the supernatant was subjected to extraction for 120min at room temperature (25°C) using a stir bar coated with polydimethylsiloxane. After the extraction, the analyte was desorbed from the stir bar by LD using acetonitrile. Then, the liquid sample was analyzed by CS-LC–MS with SPE. The average recoveries from laboratory feed samples spiked with OP and NP at 20ngg−1were 99.5 and 103.8%, respectively, with correction using the added surrogate standards. The limits of quantification were 1ngg−1for OP and 5ngg−1for NP in feed sample. The measurement of OP and NP in commercial laboratory animal feed samples resulted in the detection of sub ngg−1NP