Skopp Sonja, Oehme Michael, Fürst Peter
Organic Analytical Chemistry, University of Basel, Switzerland.
J Environ Monit. 2002 Jun;4(3):389-94. doi: 10.1039/b200133k.
High resolution gas chromatography (HRGC) coupled to quadrupole negative ion chemical ionization (NICI) mass spectrometry (MS) was used to investigate congener patterns, levels and enantiomer distribution of selected toxaphene congeners (#26, #41, #44, #50, #63, B7-1453) in human milk from Germany. #50 and #26 were the most abundant congeners. Furthermore, the identification of B7-1453, B8-1412, #41, #42, #44 and #63 was possible. Levels for the sum of #26, #41, #44 and #50 ranged from 7 to 24 microg kg(-1) milk fat and contributed between 2 and 9% to the total burden of investigated organochlorines such as selected compounds of the chlordane group, HCH, DDT and polychlorinated biphenyls (PCB). Capillaries coated with heptakis-(2,3,6-O-tert-butyldimethylsilyl)-beta-cyclodextrin (TBDMS-CD) or octakis-(2,3,6-tri-O-ethyl)-gamma-cyclodextrin (TEG-CD) were used for the enantioselective separations. Enantiomer ratios (ER) and enantiomer fractions (EF) of the abundant toxaphene congeners #26 and #50 as well as of B7-1453, #41 and #63 were determined. Greatest deviations from a racemic composition in individual human milk samples were found for #41 (1.54-2.37), #50 (1.37-1.72) and #63 (0.53-0.71) whereas ERs for #26 were close to 1. Compared to wildlife biota such as fish and raptors ER changes were more pronounced in human milk but comparable to human adipose tissue.
采用高分辨率气相色谱(HRGC)与四极杆负离子化学电离(NICI)质谱(MS)联用技术,对德国母乳中选定的毒杀芬同系物(#26、#41、#44、#50、#63、B7 - 1453)的同系物模式、含量及对映体分布进行了研究。#50和#26是含量最高的同系物。此外,还成功鉴定出了B7 - 1453、B8 - 1412、#41、#42、#44和#63。#26、#41、#44和#50的总量在7至24微克/千克乳脂肪之间,占所研究有机氯总量的2%至9%,这些有机氯包括氯丹类、六氯环己烷、滴滴涕和多氯联苯(PCB)的选定化合物。涂有七(2,3,6 - O - 叔丁基二甲基硅基)-β - 环糊精(TBDMS - CD)或八(2,3,6 - 三 - O - 乙基)-γ - 环糊精(TEG - CD)的毛细管用于对映体选择性分离。测定了含量丰富的毒杀芬同系物#26和#50以及B7 - 1453、#41和#63的对映体比率(ER)和对映体分数(EF)。在个体母乳样本中,发现#41(1.54 - 2.37)、#50(1.37 - 1.72)和#63(0.53 - 0.71)与外消旋组成的偏差最大,而#26的ER接近1。与鱼类和猛禽等野生动物生物群相比,母乳中的ER变化更为明显,但与人体脂肪组织相当。