Vetter Walter, Schlatterer Jörg, Gleixner Gerd
University of Hohenheim, Institute of Food Chemistry, Garbenstrasse 28, D-70599 Stuttgart, Germany.
J Chromatogr A. 2006 Mar 31;1110(1-2):165-70. doi: 10.1016/j.chroma.2006.01.064. Epub 2006 Feb 3.
The carbon stable isotope ratio (delta(13)C value) of an environmentally-relevant Toxaphene congener in technical products and a biological sample from a remote region was in the focus of this work. For this reason, the major octachlorobornane residue of the multicomponent pesticide Toxaphene in biological samples, 2-endo,3-exo,5-endo,6-exo,8,8,10,10-octachlorobornane (B8-1413 or P26), was quantitatively enriched from two technical Toxaphene mixtures (Toxaphene and Melipax) in duplicates as well as from an Antarctic Weddell seal sample. Normal phase followed by reversed-phase high-performance liquid chromatography (HPLC) with three columns, respectively, coupled in series was used for this purpose. Four of the five fractionated samples fulfilled the requirement of an interference-free GC-elution for subsequent determination of the delta(13)C value by gas chromatography interfaced to an isotope ratio mass spectrometer (GC-IRMS). B8-1413 in Toxaphene (n=1) was more depleted in (12)C than in Melipax (n=2), which agrees with previous results obtained for the entire mixtures. The B8-1413 isolate from a Weddell seal sample from the Antarctic showed a delta(13)C value between the two technical products. Although a source appointment to the one or the other product was not possible, this example indicates that long range transport to the Antarctic and by uptake and food-chain bioaccumulation of B8-1413 in seals did not change the delta(13)C value significantly. The observed differences in one duplicate sample indicate that statistic evaluation of samples used for isotope ratio MS measurements is an important issue.
技术产品中与环境相关的毒杀芬同系物以及来自偏远地区的生物样品的碳稳定同位素比(δ(13)C值)是本研究的重点。因此,从两种技术毒杀芬混合物(毒杀芬和Melipax)以及一份南极威德尔海豹样品中,对多组分农药毒杀芬在生物样品中的主要八氯冰片烷残留物2-内型,3-外型,5-内型,6-外型,8,8,10,10-八氯冰片烷(B8-1413或P26)进行了两次重复定量富集。为此分别使用串联三根色谱柱的正相随后反相高效液相色谱(HPLC)。五个分级分离样品中的四个满足了后续通过与同位素比质谱仪联用的气相色谱法(GC-IRMS)测定δ(13)C值时无干扰GC洗脱的要求。毒杀芬中的B8-1413(n = 1)比Melipax中的(n = 2)贫化更多的(12)C,这与之前对整个混合物获得的结果一致。从南极威德尔海豹样品中分离出的B8-1413的δ(13)C值介于两种技术产品之间。虽然无法确定其来源是这一种还是另一种产品,但这个例子表明,B8-1413远距离传输到南极并通过海豹摄取和食物链生物累积后,其δ(13)C值没有显著变化。在一个重复样品中观察到的差异表明,用于同位素比质谱测量的样品的统计评估是一个重要问题。