Wang Dongli, Miao Xiusheng, Li Qing X
Department of Molecular Biosciences and Bioengineering, University of Hawaii at Manoa, Honolulu, HI 96822, USA.
Arch Environ Contam Toxicol. 2008 Feb;54(2):211-8. doi: 10.1007/s00244-007-9016-2. Epub 2007 Aug 25.
A gas chromatography/ion trap mass spectrometry method was developed for analysis of organochlorine pesticides (OCPs) in coral samples, which were extracted with accelerated solvent extraction (ASE) and cleaned up on a sulfuric acid-modified silica gel column. The optimal ASE conditions were found to be 100 degrees C and 2000 psi, with a mixture of acetone and methylene chloride (1:1, v/v). The target analytes include hexachlorocyclohexanes (HCHs, specifically, alpha-, beta-, gamma-, and delta-HCH isomers), heptachlor, and hexachlorobenzene (HCB), o,p'-, p,p'-dichlorodiphenyltrichloroethane (o,p'-, p,p'-DDT), o,p'-, p,p'-dichlorodiphenyl-dichloroethylene (o,p'-, p,p'-DDE), and o,p'-, p,p'-dichlorodiphenyldichloroethane (o,p'-, p,p'-DDD). Standard sand samples were used as an alternative matrix spiked with OCP standards to determine the method precision and accuracy. Average recoveries of OCPs ranged from 82% to 102%, with relative standard deviations (RSDs) of 3%-6%, at a level of 10 ng/g and from 50% to 68%, with RSDs of 13%-19% at a level of 2 ng/g. The developed method was applied for analysis of OCPs in coral samples collected from Tern Island and Bikini Atoll in the Pacific Ocean. The concentrations of HCB were 7-26 pg/g dry weight in the samples from Bikini Atoll and 3-45 pg/g in those from Tern Island, and heptachlor concentrations were 208-2200 and 44-104 pg/g in the coral samples from Bikini Atoll and Tern Island, respectively. (summation operator)HCH (sum of alpha-, beta-, gamma-, and delta-HCH) were 8-82 pg/g in Bikini Atoll coral and 86-629 pg/g in Tern island coral, and (summation operator)DDT (sum of o,p'-, p,p'-DDD, o,p'-, p,p'-DDE, and o,p'- p,p'-DDT) were 80-212 pg/g in Bikini Atoll coral and 593-3165 pg/g in Tern Island coral. The results suggest that coral is a viable indicator species for pollution monitoring, which pollutants and their concentrations may be related to dated carbonate layers.
建立了一种气相色谱/离子阱质谱法，用于分析珊瑚样品中的有机氯农药（OCPs）。样品采用加速溶剂萃取（ASE）提取，并在硫酸改性硅胶柱上进行净化。最佳ASE条件为100℃和2000 psi，萃取剂为丙酮和二氯甲烷的混合溶液（1:1，v/v）。目标分析物包括六氯环己烷（HCHs，具体为α-、β-、γ-和δ-HCH异构体）、七氯、六氯苯（HCB）、o,p'-、p,p'-二氯二苯三氯乙烷（o,p'-、p,p'-DDT）、o,p'-、p,p'-二氯二苯二氯乙烯（o,p'-、p,p'-DDE）和o,p'-、p,p'-二氯二苯二氯乙烷（o,p'-、p,p'-DDD）。使用标准砂样作为替代基质，加入OCP标准品以确定方法的精密度和准确度。OCPs在10 ng/g水平下的平均回收率为82%至102%，相对标准偏差（RSDs）为3% - 6%；在2 ng/g水平下的平均回收率为50%至68%，RSDs为13%至19%。所建立的方法应用于分析从太平洋的特恩岛和比基尼环礁采集的珊瑚样品中的OCPs。比基尼环礁样品中HCB的浓度为7 - 26 pg/g干重，特恩岛样品中为3 - 45 pg/g；比基尼环礁珊瑚样品中七氯的浓度为208 - 2200 pg/g，特恩岛珊瑚样品中为44 - 104 pg/g。比基尼环礁珊瑚中∑HCH（α-、β-、γ-和δ-HCH的总和）为8 - 82 pg/g，特恩岛珊瑚中为86 - 62⑨ pg/g；比基尼环礁珊瑚中∑DDT（o,p'-、p,p'-DDD、o,p'-、p,p'-DDE和o,p'-、p,p'-DDT的总和）为80 - 212 pg/g，特恩岛珊瑚中为593 - 3165 pg/g。结果表明，珊瑚是污染监测的可行指示物种，其污染物及其浓度可能与年代久远的碳酸盐层有关。
