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土壤中典型人工甜味剂的前处理方法优化及高效液相色谱-串联质谱分析
  • 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]南开大学,环境污染过程与基准教育部重点实验室,天津300071
  • 相关基金:国家杰出青年基金项目(41225014); 国家“973”计划项目(2014CB441104)
中文摘要:

优化了同时提取土壤中4种典型人工甜味剂的前处理与净化方法,并结合高效液相色谱-串联质谱(HPLCMS/MS)技术,建立了一种快速高效的分析方法。样品采用25 mL0.01 mol/L醋酸-醋酸钠溶液(pH4)提取2次,每次提取20 min;萃取样品进一步采用CNW Poly-Sery PWAX固相萃取小柱净化浓缩;最后采用HPLC-MS/MS进行测定。在干燥土壤中添加1、10、100μg/kg标准品时,4种甜味剂的平均回收率为86.5%-105%,日内精密度(RSD)≤5.94%,日间精密度(RSD)≤6.53%;在1-100μg/kg范围内的线性关系良好(r2〉0.995);方法的检出限为0.01-0.21μg/kg,定量限为0.03-0.70μg/kg。利用该方法对天津某污水灌溉的农田土壤进行了分析测定,结果表明该方法快捷可靠,可用于土壤中人工甜味剂的环境调查。

英文摘要:

The sample pretreatment method for the determination of four typical artificial sweeteners (ASs) including sucralose, saccharin, cyclamate, and acesulfame in soil by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was optimized. Different conditions of extraction, including four extractants ( methanol, acetonitrile, acetone, deionized water), three kinds of ionic strength of sodium acetate solution (0. 001, 0.01, 0. 1 mol/L), four pH values (3, 4, 5 and 6) of 0.01 mol/L acetate-sodium acetate solution, four set durations of extraction (20, 40, 60, 120 min) and number of extraction times ( 1, 2, 3, 4 times) were compared. The optimal sample pretreatment method was finally set up. The samples were extracted twice with 25 mL 0.01 mol/L sodium acetate solution (pH 4) for 20 min per cycle. The extracts were combined and then purified and concentrated by CNW Poly-Sery PWAX cartridges with methanol containing I mmol/L tris (hydroxymethyl) amino methane (Tris) and 5% (v/v) ammonia hydroxide as eluent. The analytes were determined by HPLC- MS/MS. The recoveries were obtained by spiked soil with the four artificial sweeteners at 1, 10, 100 μg/kg (dry weight), separately. The average recoveries of the analytes ranged from 86.5% to 105%. The intra-day and inter-day precisions expressed as relative standard deviations (RSDs) were in the range of 2.56%-5.94% and 3.99%-5.53%, respectively. Good linearities ( r^2〉0. 995) were observed between 1-100 μg/kg (dry weight) for all the compounds. The limits of detection were 0.01-0.21μg/kg and the limits of quantification were 0.03-0.70μg/kg for the analytes. The four artificial sweeteners were determined in soil samples from farmland contaminated by wastewater in Tianjin. This method is rapid, reliable, and suitable for the investigation of artificial sweeteners in soil.

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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