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

发布时间：2018-03-23 05:17

  本文选题：凝胶渗透色谱　切入点：气相色谱-负化学电离源-质谱　出处：《化学通报》2015年02期 　论文类型：期刊论文

【摘要】：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)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),空白样品还额外加入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%±14.0%、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/m L。应用本方法对人乳样品进行检测,均没有检出CB-77,81,169、BDE-154,85、syn-DP、anti-DP。∑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:0.11~0.22、4.9~7.9、0.0037~0.0056和0.0053~0.021ng/m L。
[Abstract]:The method of gel permeation chromatography (GPC) for degreasing was established. Gas chromatography-negative chemical ionization source-mass spectrometry (GC-NCI-MS) method for the determination of PBDEsN, DKN, including syn-DP and anti-DPN, HBB and PCBsof polychlorinated biphenyl in human milk. The internal standard 13C12-BDE-139C12-BDE-209C10-syn-DP13C12-PCBsn 13C12-CB-817712121231181241051261661571691890 was added to the human milk samples, and the blank sample was also added to the sample with the amount of 13C12-BDE-13C12BE-20C10-syn-D13C12-PCBsn. After adding PBT and HBB, the protein was removed by adding acid. After liquid-liquid extraction, GPC degreasing, acid silica gel column purification, The recoveries of 13C12-BDE-13C12-BDE-209C10-syn-DPn13C12-PCBs in human milk samples were 112.9% 卤14.0G 99.3% 卤12.7R 80.5% 卤17.9% 卤2.4% 卤2.4respectively. The recoveries of PBT and HBB in blank samples were 102.8% 卤18.0% and 88.1% 卤14.4.The detection limits of each halogen compounds were 0.33~333.3pg/m L. There were no detectable concentrations of CB-77, 81169, BDE-154N, 85-syn-DPU anti-DP. 鈭，

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