本文選題：凝膠滲透色譜　切入點(diǎn)：氣相色譜-負(fù)化學(xué)電離源-質(zhì)譜　出處：《化學(xué)通報(bào)》2015年02期 　論文類型：期刊論文

【摘要】：建立了用凝膠滲透色譜(GPC)去脂、氣相色譜-負(fù)化學(xué)電離源-質(zhì)譜(GC-NCI-MS)測定人乳中多溴聯(lián)苯醚(PBDEs)、德克隆(DP,包括syn-DP和anti-DP)、五溴甲苯(PBT)、六溴苯(HBB)和多氯聯(lián)苯(PCBs)的方法。人乳樣品中加入內(nèi)標(biāo)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),空白樣品還額外加入PBT和HBB,經(jīng)過加酸去蛋白質(zhì)、液液萃取、GPC去脂、酸性硅膠柱凈化后,定量測定。人乳樣品中13C12-BDE-139、13C12-BDE-209、13C10-syn-DP、13C12-PCBs的加標(biāo)回收率分別為112.9%±14.0%、99.3%±12.7%、80.5%±17.9%、64.6%±2.4%,空白樣品中PBT和HBB的加標(biāo)回收率分別為102.8%±18.0%和88.1%±14.4%,各鹵代化合物檢出限范圍為0.33~333.3pg/m L。應(yīng)用本方法對人乳樣品進(jìn)行檢測,均沒有檢出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濃度范圍分別為: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% 鹵14.0G 99.3% 鹵12.7R 80.5% 鹵17.9% 鹵2.4% 鹵2.4respectively. The recoveries of PBT and HBB in blank samples were 102.8% 鹵18.0% and 88.1% 鹵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，

本文編號：1652052