复合层析柱净化-气相色谱-负化学源质谱法测定海洋沉积物中多溴联苯醚

O658; 采用去活硅胶-酸化硅胶-去活硅胶-弗罗里硅土-无水硫酸钠填装的复合层析柱,结合气相色谱-负化学源质谱法(GC-NCI/MS)对海洋沉积物样品中的13种多溴联苯醚(PBDEs)进行分析检测.样品用正己烷-二氯甲烷(3:1,v/v)混合溶剂进行超声提取,提取液经复合层析柱净化及正己烷-二氯甲烷(3:1,v/v)混合溶剂洗脱后,利用GC-NCI/MS的选择离子监测(SIM)模式分析测定13种PBDEs.对比分析了复合层析柱中不同填料、不同洗脱剂以及不同洗脱体积对PBDEs净化效果的影响,并对GC-NCI/MS分析条件进行优化处理.最终13种PBDEs在0.1～20μg/L内线性关系良好,...

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Published inSepu Vol. 41; no. 6; pp. 535 - 542
Main Authors 董婧妍, 宋素平, 孙秀梅, 金衍健, 郝青, 朱剑, 李铁军
Format Journal Article
LanguageChinese
English
Published No. 457, Zhongshan Road, Shahekou District, Dalian City, Liaoning Province 浙江海洋大学海洋与渔业研究所,浙江 舟山316021%浙江省海洋水产研究所,浙江省海洋渔业资源可持续利用技术研究重点实验室,浙江 舟山316021 08.06.2023
Editorial board of Chinese Journal of Chromatography
Subjects
a
复合层析柱净化
气相色谱-负化学源质谱
多溴联苯醚
沉积物
Online AccessGet full text
ISSN1000-8713
1872-2059
DOI10.3724/SP.J.1123.2022.10006

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Abstract O658; 采用去活硅胶-酸化硅胶-去活硅胶-弗罗里硅土-无水硫酸钠填装的复合层析柱,结合气相色谱-负化学源质谱法(GC-NCI/MS)对海洋沉积物样品中的13种多溴联苯醚(PBDEs)进行分析检测.样品用正己烷-二氯甲烷(3:1,v/v)混合溶剂进行超声提取,提取液经复合层析柱净化及正己烷-二氯甲烷(3:1,v/v)混合溶剂洗脱后,利用GC-NCI/MS的选择离子监测(SIM)模式分析测定13种PBDEs.对比分析了复合层析柱中不同填料、不同洗脱剂以及不同洗脱体积对PBDEs净化效果的影响,并对GC-NCI/MS分析条件进行优化处理.最终13种PBDEs在0.1～20μg/L内线性关系良好,相关系数(r2)>0.995(BED-209,r2>0.99),定量限(S/N=10)为0.002～0.126μg/kg.以海洋沉积物样品为基质,13种PBDEs在0.2、1.0、4.0μg/kg 3个加标水平下的平均回收率分别为85.3％～101.3％、84.8％ ～113.6％、86.3％ ～94.7％,相对标准偏差分别为4.4％ ～14.0％、0.4％ ～4.9％、1.9％ ～6.6％.结果表明,该方法的灵敏度和准确度高,精密度良好.应用本方法对所采集的海洋沉积物样品进行分析检测,结果显示13种PBDEs均有不同程度的检出,其中BDE-209含量较高,最高达60.49μg/kg.实际样品检测结果表明本方法适用于海洋沉积物样品中PBDEs的准确定性定量分析.
AbstractList 采用去活硅胶-酸化硅胶-去活硅胶-弗罗里硅土-无水硫酸钠填装的复合层析柱,结合气相色谱-负化学源质谱法(GC-NCI/MS)对海洋沉积物样品中的13种多溴联苯醚(PBDEs)进行分析检测。样品用正己烷-二氯甲烷(3∶1, v/v)混合溶剂进行超声提取,提取液经复合层析柱净化及正己烷-二氯甲烷(3∶1, v/v)混合溶剂洗脱后,利用GC-NCI/MS的选择离子监测(SIM)模式分析测定13种PBDEs。对比分析了复合层析柱中不同填料、不同洗脱剂以及不同洗脱体积对PBDEs净化效果的影响,并对GC-NCI/MS分析条件进行优化处理。最终13种PBDEs在0.1~20 μg/L内线性关系良好,相关系数(r2)>0.995(BED-209, r2>0.99),定量限(S/N=10)为0.002~0.126 μg/kg。以海洋沉积物样品为基质,13种PBDEs在0.2、1.0、4.0 μg/kg 3个加标水平下的平均回收率分别为85.3%~101.3%、84.8%~113.6%、86.3%~94.7%,相对标准偏差分别为4.4%~14.0%、0.4%~4.9%、1.9%~6.6%。结果表明,该方法的灵敏度和准确度高,精密度良好。应用本方法对所采集的海洋沉积物样品进行分析检测,结果显示13种PBDEs均有不同程度的检出,其中BDE-209含量较高,最高达60.49 μg/kg。实际样品检测结果表明本方法适用于海洋沉积物样品中PBDEs的准确定性定量分析。
O658; 采用去活硅胶-酸化硅胶-去活硅胶-弗罗里硅土-无水硫酸钠填装的复合层析柱,结合气相色谱-负化学源质谱法(GC-NCI/MS)对海洋沉积物样品中的13种多溴联苯醚(PBDEs)进行分析检测.样品用正己烷-二氯甲烷(3:1,v/v)混合溶剂进行超声提取,提取液经复合层析柱净化及正己烷-二氯甲烷(3:1,v/v)混合溶剂洗脱后,利用GC-NCI/MS的选择离子监测(SIM)模式分析测定13种PBDEs.对比分析了复合层析柱中不同填料、不同洗脱剂以及不同洗脱体积对PBDEs净化效果的影响,并对GC-NCI/MS分析条件进行优化处理.最终13种PBDEs在0.1～20μg/L内线性关系良好,相关系数(r2)>0.995(BED-209,r2>0.99),定量限(S/N=10)为0.002～0.126μg/kg.以海洋沉积物样品为基质,13种PBDEs在0.2、1.0、4.0μg/kg 3个加标水平下的平均回收率分别为85.3％～101.3％、84.8％ ～113.6％、86.3％ ～94.7％,相对标准偏差分别为4.4％ ～14.0％、0.4％ ～4.9％、1.9％ ～6.6％.结果表明,该方法的灵敏度和准确度高,精密度良好.应用本方法对所采集的海洋沉积物样品进行分析检测,结果显示13种PBDEs均有不同程度的检出,其中BDE-209含量较高,最高达60.49μg/kg.实际样品检测结果表明本方法适用于海洋沉积物样品中PBDEs的准确定性定量分析.
Author 董婧妍
郝青
孙秀梅
宋素平
朱剑
金衍健
李铁军
AuthorAffiliation 浙江海洋大学海洋与渔业研究所,浙江 舟山316021%浙江省海洋水产研究所,浙江省海洋渔业资源可持续利用技术研究重点实验室,浙江 舟山316021
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Author_FL SONG Suping
SUN Xiumei
ZHU Jian
HAO Qing
LI Tiejun
JIN Yanjian
DONG Jingyan
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Issue 6
Keywords 复合层析柱净化
气相色谱-负化学源质谱
多溴联苯醚
沉积物
Language Chinese
English
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Snippet O658; 采用去活硅胶-酸化硅胶-去活硅胶-弗罗里硅土-无水硫酸钠填装的复合层析柱,结合气相色谱-负化学源质谱法(GC-NCI/MS)对海洋沉积物样品中的13种多溴联苯醚(PBDEs)进行...
采用去活硅胶-酸化硅胶-去活硅胶-弗罗里硅土-无水硫酸钠填装的复合层析柱,结合气相色谱-负化学源质谱法(GC-NCI/MS)对海洋沉积物样品中的13种多溴联苯醚(PBDEs)进行分析检...
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Title 复合层析柱净化-气相色谱-负化学源质谱法测定海洋沉积物中多溴联苯醚
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