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皮革中游离烷基酚和乙氧基化烷基酚的测定 。

Determination of free and ethoxylated alkylphenols in leather with gas chromatography-mass spectrometry.

机构信息

Quality & Technical Supervision and Inspection Institute of Zhejiang Province, Hangzhou, China.

出版信息

J Chromatogr A. 2010 Dec 10;1217(50):7914-20. doi: 10.1016/j.chroma.2010.10.063. Epub 2010 Oct 21.

Abstract

An analytical approach was developed to determine nonylphenol (NP), octylphenol (OP), nonylphenol ethoxylates (NPEO(n)) and octylphenol ethoxylates (OPEO(n)) in leather samples involving the conversion of NPEO(n) and OPEO(n) into the corresponding NP and OP. The four targets were extracted from samples using ultrasonic-assisted acetonitrile extraction. NP and OP in the extracts were directly isolated with hexane and quantitatively determined with 4-n-nonylphenol as internal standard by gas chromatography-mass spectrometry (GC-MS). For NPEO(n) and OPEO(n) in the extracts, they were first converted into NP and OP with aluminum triiodide as cleavage agent, and the yielded NP and OP were determined by GC-MS. The contents of NPEO(n) and OPEO(n) were calculated by normalizing to NPEO(9) and OPEO(9), respectively. This method was properly validated and the real sample tests revealed the pollution significance of leather by NPEO(n) and OPEO(n).

摘要

建立了一种分析方法,用于测定皮革样品中的壬基酚(NP)、辛基酚(OP)、壬基酚聚氧乙烯醚(NPEO(n))和辛基酚聚氧乙烯醚(OPEO(n)),涉及将 NPEO(n) 和 OPEO(n) 转化为相应的 NP 和 OP。采用超声辅助乙腈提取法从样品中提取这四种目标物。用正己烷直接从提取物中分离 NP 和 OP,并用 4-正壬基酚作为内标,通过气相色谱-质谱联用(GC-MS)定量测定。对于提取物中的 NPEO(n) 和 OPEO(n),先用三碘化铝作为裂解剂转化为 NP 和 OP,然后用 GC-MS 测定生成的 NP 和 OP。通过将 NPEO(n) 和 OPEO(n) 的含量归一化为 NPEO(9) 和 OPEO(9),分别计算其含量。该方法经过适当验证,实际样品测试结果表明,NPEO(n) 和 OPEO(n) 对皮革造成了污染。

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