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凝固漂浮有机液滴-分散液液微萃取-高效液相色谱-串联质谱法测定海水中苯并三唑类紫外线过滤剂
  • ISSN号:1000-8713
  • 期刊名称:《色谱》
  • 时间:0
  • 分类:O658[理学—分析化学;理学—化学]
  • 作者机构:[1]中国科学院大连化学物理研究所,辽宁大连116023, [2]霍尼韦尔综合科技(中国)有限公司,上海201203
  • 相关基金:国家高技术研究发展计划(“863”计划)项目(2013AA065203); 国家自然科学基金项目(21277139)
中文摘要:

建立了海水中7种苯并三唑类紫外线过滤剂的凝固漂浮有机液滴-分散液液微萃取-高效液相色谱-串联质谱分析方法。优化后的萃取实验条件:20μL十二醇为萃取溶剂,400μL甲醇为分散溶剂,NaCl质量分数为8%,pH小于6,涡旋振荡时间2 min。目标化合物经Hypersil GOLD色谱柱(150 mm×2.1 mm,5μm)结合甲醇-水梯度洗脱分离后,用正离子多反应监测模式进行质谱分析。在较宽的线性范围内,7种化合物的线性相关系数(r2)均大于0.99;基质加标回收率为68.3%-127.5%,相对标准偏差为0.9%-15.2%,方法的检出限为0.001-0.090μg/L,定量限为0.003-0.300μg/L。将建立的方法用于大连8个海滨浴场海水中苯并三唑类紫外线过滤剂的测定,部分浴场海水有不同程度的检出。该方法简便、快速、环境友好、灵敏度高,可用于海水中苯并三唑类紫外线过滤剂的分析检测。

英文摘要:

A novel dispersive liquid-liquid microextraction method based on solidification of floating organic droplets (DLLME-SFO) technique was developed for the determination of seven benzotriazole ultraviolet (UV) stabilizers in seawater samples by high performance liquid chromatography with tandem mass spectrometry. The optimal liquid-liquid microextraction experiment conditions were as follows: 20 μL of l-dodecanol as extraction solvent, 400 μL of methanol as dispersive solvent, 8% ( mass percentage) NaC1, pH of the sample below 6, vortex oscillation extraction time in 2 rain. The separation of target compounds was achieved by combining a Hypersil GOLD analytical colunm ( 150 mm×2. 1 mm, 5 μm) with methanol-water as mobile phase with gradient elution program. Quantitative determination by ESI-MS/MS was achieved using positive ion mode with multiple reaction monitoring mode. The proposed method showed good linearity with the correlation coefficients all above 0.99. The blank samples were spiked at three levels and the average recoveries of target compounds ranged from 68.3% to 127.5% with the RSDs from 0.9% to 15.2%. The limits of detection (LODs) and limits of quantification (LOQs) of the method for the seven target compounds were in the ranges of 0. 001- 0. 090 μg/L and 0. 003- 0. 300 μg/L, respectively. The developed method was successfully applied for the analysis of the UV stabilizers in seawater at Dalian seashores, and some of the benzotriazoles were detected. The method is simple, rapid, environment friendly, highly sensitive and suitable for rapid analysis of benzotriazole UV stabilizers in seawater.

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期刊信息
  • 《色谱》
  • 北大核心期刊(2011版)
  • 主管单位:中国科学技术协会
  • 主办单位:中国化学会 中国科学院大连化学物理研究所
  • 主编:张玉奎
  • 地址:大连市中山路457号
  • 邮编:116023
  • 邮箱:sepu@dicp.ac.cn
  • 电话:0411-84379021
  • 国际标准刊号:ISSN:1000-8713
  • 国内统一刊号:ISSN:21-1185/O6
  • 邮发代号:8-43
  • 获奖情况:
  • 1998年获中国科学院科学出版基金择优支持(1998-2...,2001年获第四届中国科学院优秀期刊二等奖,2002年获第三届中国科协优秀期刊三等奖,连续多年被评为辽宁省一级期刊
  • 国内外数据库收录:
  • 俄罗斯文摘杂志,美国化学文摘(网络版),波兰哥白尼索引,荷兰文摘与引文数据库,美国生物医学检索系统,美国剑桥科学文摘,日本日本科学技术振兴机构数据库,中国中国科技核心期刊,中国北大核心期刊(2004版),中国北大核心期刊(2008版),中国北大核心期刊(2011版),中国北大核心期刊(2014版),英国英国皇家化学学会文摘,中国北大核心期刊(2000版)
  • 被引量:26730