摘要
建立了气相色谱串联质谱法鉴别多氯联苯二代污染物羟基多氯联苯的方法,并用于水产品中羟基多氯联苯的分析。在60℃下,羟基多氯联苯经硅烷化衍生40min,在气相色谱三重四级杆串联质谱仪全扫描模式（Fullscanmode）下进行扫描,得到一级质谱全扫描图谱,确定3-羟基-多氯联苯101（3-OH-PCB101）、4-羟基-多氯联苯106（4-OH-PCB106）、4-羟基-多氯联苯112（4-OH-PCB112）等7种衍生化合物丰度最高的碎片离子,以此碎片离子为母离子,在二级质谱多反应监测模式（MRM）下进行扫描,得到二级质谱全扫描图谱,确定母离子产生的丰度最高的特征子离子,以此对应的离子对及其比例对化合物进行定性分析,分别得到7种羟基多氯联苯衍生物的一级、二级质谱图,通过串联质谱法对每种目标化合物进行定量分析,仪器检出限范围为0.02-0.14μg/L,定量检出限为0.09-0.48μg/L。将本方法用于水产品中羟基多氯联苯的鉴别,结果满意。
Gas chromatography-tandem mass spectrometry was adopted to identify the hydroxylated metabolites of polychlorinated biphenyls and analyze the target compounds in fishery products. After the silylation derivatizaiton at 60 ℃ for 40 min, the MS spectrum of derivatives was obtained by GC/MS/MS under fullscan mode, and the fragment ions with the highest relative abundance were identified as m/z 399, 399, 399, 399, 399, 448 and 469, respectively which were defined as the precursor ion for product ion scan. The MS/MS spectrum was obtained under multiple reaction mode （ MRM ） by GC/MS/MS. And the product ions corresponded with the precursor ions were m/z 364, 364, 364, 364, 364, 433 and 434, respectively. The target compounds can be identified accurately by GC/MS/MS. In the present study, we took seven hydroxylated polychlorinated biphenyls as target compounds including 3-OH-PCB101 , 4-OH-PCB106 , 4-OH-PCB112 , 4＆#39;-OH-PCB101 , 3-OH-PCB118 , 3-OH-PCB138 and 3-OH-PCB180 . According to the identification method stated as above, the MS and MS/MS spectra of seven compounds were obtained. The compounds can be qualified and quantified by the identification method. The limits of detection ranged from 0. 02 to 0. 14 μg/L, and the limits of quantification ranged from 0. 09 to 0. 48 μg/L. The method has been applied to identify the hydroxylated polychlorinated biphenyls in fishery products.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2014年第11期1640-1645,共6页
Chinese Journal of Analytical Chemistry
基金
中国水产科学研究院东海水产研究所中央级公益性科研院所基本科研业务费支持(No.2011M12)~~
关键词
气相色谱串联质谱法
多氯联苯
二代污染物
羟基多氯联苯
Gaschromatography-tandemmassspectrometry
Polychlorinatedbiphenyls
Metabolized pollutants
Hydroxylated polychlorinated biphenyls
作者简介
E-mail：hdm2001@126．com
