| 孙一鸣,徐萌,李光耀,何畅,王英,田旸,金军.化学通报,2015,78(2):170-176. |
| 凝胶渗透色谱-气相色谱-质谱法测定人乳中卤代有机化合物 |
| Determination of Halogenated Organic Compounds in Human Milk by Gel Permeation Chromatography-Gas Chromatography-Mass Spectrometry |
| 投稿时间：2014-02-24 修订日期：2014-04-07 |
| DOI： |
| 中文关键词: 凝胶渗透色谱 气相色谱-负化学电离源-质谱 人乳 卤代有机化合物 |
| 英文关键词:Gel permeation chromatography Gas chromatography-Negative chemical ionization-Mass spectrometry human milk halogenated organic compounds |
| 基金项目:教育部新世纪优秀人才支持计划(NCET-10-0106)、中央民族大学985工程(MUC985-9)和高等学校学科创新引智计划项目(B0844)资助 |
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| 中文摘要: |
| 本研究建立了用凝胶渗透色谱（GPC）去脂，气相色谱-负化学电离源-质谱（GC-NCI-MS）法测定人乳中多溴联苯醚（PBDEs），德克隆（DP，包括syn-DP 和anti-DP），五溴甲苯（PBT），六溴苯（HBB）和多氯联苯（PCBs）的方法。人乳样品中加入内标13C12-BDE-139、13C12-BDE-209、13C10-syn-DP、13C12-PCBs（13C12-CB-81,77,123,118,114,105,126,167,156,157,169,189），空白样品额外还加入PBT和HBB，经过加酸去蛋白质、液液萃取、GPC去脂、酸性硅胶柱净化后，定量测定。人乳样品中13C12-BDE-139、13C12-BDE-209、13C10-syn-DP、13C12-PCBs的加标回收率分别为112.9?Ee14.0%、99.3%±12.7%、80.5%±17.9%、64.6%±2.4%，空白样品中PBT和HBB的加标回收率分别为102.8%±18.0%和88.1%±14.4%，各卤代化合物检出限范围为0.33-333.3pg/mL。应用本方法对人乳样品进行检测，CB-77,81,169、BDE-154,85、syn-DP、anti-DP均无检出。∑9PCBs（CB-123,118,114,105,126,167,156,157,189）、∑8PBDEs（BDE-28,47,100,99,153,183,190,209）、PBT、HBB浓度范围分别为：0.11~0.22ng/mL、4.9~7.9ng/mL、0.0037~0.0056 ng/mL、0.0053~0.021ng/mL。 |
| 英文摘要: |
| A method, using Gel Permeation Chromatography(GPC) to remove lipid and using Gas Chromatography-Negative Chemical Ionization-Mass Spectrometry(GC-NCI-MS) to detect halogenated compounds such as Polybrominated diphenylethers (PBDEs), Polychlorinated biphenyls(PCBs), Dechlorane plus(DP, including syn-DP and anti-DP), Pentabromotoluene (PBT) and Hexabromobenzene (HBB), was developed in this study. The blank and human milk samples were spiked with 13C12-BDE-139, 13C12-BDE-209, 13C10-syn-DP, 13C12-PCBs (13C12-CB-81,77,123,118,114,105,126,167, 156,157, 169,189) as internal standard, also PBT, HBB were added into the blank samples. All the samples were dealt with hydrochloric acid to denature protein before extracting, then the lipid was mostly removed by gel permeation chromatography. Samples were further cleaned up by a silica/sulfuric acid column before determined. The recoveries of 13C12-BDE-139, 13C12-BDE-209, 13C10-syn-DP, 13C12-PCBs in human milk samples were 112.9?Ee14.0%, 99.3%±12.7%, 80.5%±17.9%, 64.6%±2.4%, respectively, the recoveries of PBT and HBB in blank samples were 102.8%±18.0% and 88.1%±14.4%. The limits of detection of the halogenated organic compounds were ranged from 0.33-333.3 ng/mL. CB-81,77,169, BDE-154,85, syn-DP, anti-DP were not detected in any blank or human milk samples, the concentrations of ∑9PCBs (CB-123,118,114,105,126, 167,156,157,189), ∑8 PBDEs(BDE-28,47,100,99,153,183, 190,209), PBT, HBB were0.11~0.22ng/mL, 4.9~7.9ng/mL, 0.0037~0.0056 ng/mL, 0.0053~0.021ng/mL, respectively. |
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