Headspace solid-phase micro-extraction gas chromatography-mass detection method for the determination of butyltin compounds in wines
Headspace solid-phase micro-extraction gas chromatography-mass detection method for the determination of butyltin compounds in wines
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DOI：
10.1016/s0003-2670(01)01620-8
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发表时间：
2002-04-29
影响因子：
6.2
通讯作者：
Vasconcelos, MT
中科院分区：
文献类型：
--
作者：
Azenha, M;Vasconcelos, MT
丁基锡化合物是广泛存在的污染物，在一些葡萄酒中也发现了丁基锡化合物，通过液-液萃取，然后用格氏试剂进行烷基化和气相色谱-质谱（GC-MS）分析来测定。这种萃取/衍生化方法的一个有前途的替代方案是一步四乙基硼酸酯原位乙基化/固相微萃取（SPME）方法。本文建立了葡萄酒中丁基锡化合物的SPME-GC-MS测定方法。优化的参数涉及与四甲基铵的预处理。氢氧化物、用氯化钠的基质改性、四乙基硼酸盐浓度、萃取时间和温度以及GC分离程序。评价了优化方法的分析优值（范围、检测限（LOD）和重现性）。灵敏度（范围为20-1421 kcounts mug（-1）1（-1），以Sn计）和LOD（范围为0.01-0.2 mug 1（-1），以Sn计）在很大程度上取决于待测量的丁基锡种类和葡萄酒类型。对于测试的物种（一丁基锡，二丁基锡和三丁基锡）的最高灵敏度达到波特酒样品，其次是红葡萄酒>白色葡萄酒>白色绿葡萄酒。该方法允许可接受的重复性（相对标准偏差（R.S.D.），6-8%; n = 4）和再现性（R.S.D.，8-9%; n = 3）。(C)2002 Elsevier Science B. V.保留所有权利。
Butyltin compounds are widespread contaminants which have also been found in some wines, determined by Liquid-liquid extraction followed by alkylation with a Grignard reagent and gas chromatography-mass spectrometric (GC-MS) analysis. A promising alternative to this extraction/derivatization method is the one-step tetraethylborate in situ ethylation/solid-phase micro-extraction (SPME) method. In this work, a SPME-GC-MS method for the determination of butyltin compounds in wine was optimised. The optimised parameters concerned the pre-treatment with tetramethylammonium. hydroxide, matrix modification with sodium chloride, tetraethylborate concentration, extraction time and temperature, and the GC separation program. The analytical figures of merit of the optimised method (range, limit of detection (LOD) and reproducibility) were evaluated. The sensitivity (range 20-1421 kcounts mug(-1) 1(-1) as Sn) and LOD (range, 0.01-0.2 mug 1(-1) as Sn) depended greatly on the butyltin species to be measured and on the type of wine. For the tested species (monobutyltin, dibutyltin and tributyltin) the highest sensitivities were achieved for Port wine samples, followed by red wine > white wine > white Verde wine. The method allowed acceptable repeatability (relative standard deviation (R.S.D.), 6-8%; n = 4) and reproducibility (R.S.D., 8-9%; n = 3). (C) 2002 Elsevier Science B.V. All rights reserved.