在线凝胶渗透色谱-固相萃取-气相色谱/质谱法测定吸烟者尿液中的苯并[a]芘
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- 英文论文题名：Analysis of benzo[a]pyrene in smoker urine sample by online gel permeation chromatography– solid phase extraction- gas chromatography/mass spectrometry
- 论文作者：司晓喜 ; 朱瑞芝 ; 刘志华 ; 张凤梅 ; 刘春波 ; 申钦鹏 ; 何沛 ; 缪明明 ; 杨光宇
- 英文论文作者：SI Xiao-xi ; ZHU Rui-zhi ; LIU Zhi-hua ; ZHANG Feng-mei ; LIU Chun-bo ; SHEN Qin-peng ; HE Pei ; MIAO Ming-ming ; YANG Guang-yu ; Key Lab of Tobacco Chemistry of Yunnan ; R&D Center ; China Tobacco Yunnan Industrial Co. ; Ltd.
- 年：2016
- 作者机构：云南省烟草化学重点实验室云南中烟工业有限责任公司技术中心;
- 论文关键词：在线固相萃取 ; 液相/气相二维色谱 ; 线凝胶渗透色谱 ; 气相色谱/质谱法 ; 苯并[a]芘 ; 尿液
- 英文论文关键词：Online solid phase extraction ; Comprehensive two-dimensional liquid-gas chromatography ; Gel permeation chromatography ; gas chromatography/mass spectrometry ; Benzo[a]pyrene ; Urine
- 会议召开时间：2016-12-01
- 会议录名称：中国烟草学会2016年度优秀论文汇编——烟草工业主题
- 语种：中文
- 分类号：R446.12;O657.63
- 学会代码：ZGYG
- 学会名称：中国烟草学会
- 页数：8
- 文件大小：1191k
- 原文格式：D
摘要
建立了在线凝胶渗透色谱-固相萃取-气相色谱/质谱(GPC-SPE-GC/MS)测定吸烟者尿液中的苯并[a]芘(B[a]P)方法。吸烟者尿液样品用含D12-B[a]P内标的环己烷萃取,然后经凝胶色谱柱分离,含B[a]P的馏分切割到硅胶固相萃取柱上富集,富集的B[a]P用丙酮洗脱进入气相色谱-质谱分析。该方法实现了凝胶渗透色谱、固相萃取和气相色谱/质谱的在线连接,样品无需多步骤的手动净化步骤。液相色谱使用凝胶柱,进样量提高至到200μL,样品载样量比常规微型硅胶柱提高了10倍;在线固相萃取实现了液相色谱净化后的大体积馏分切割进入气相色谱,有效提高了灵敏度。该方法在B[a]P含量为0.08-10 ng/m L范围内具有良好的线性关系,相关系数为0.9992;方法日内相对标准偏差为3.26%,日间相对标准偏差为3.87%;B[a]P的加标回收率在95.6%-97.2%;方法检出限和定量限分别为0.022ng/L和0.093ng/L。方法自动化,简单快速,灵敏度高,准确度好,实际用于吸烟者尿液中B[a]P分析结果令人满意。
A new method for the determination of benzo[a]pyrene(B[a]P) in smoker urine sampleswas developed by online gel permeation chromatography-solid phase extraction-gas chromatography/mass spectrometry(GPC-SPE-GC/MS) hyphenated system. Smoker urine samples were extracted with cyclohexane containing D12-B[a]P as internal standard. Then, the extract was separated by gel permeation chromatography, and B[a]Pfraction was cutting into thesolid phase extraction cartridge and was enriched. The enriched B[a]P was eluted by acetone, then was determined by gas chromatography- mass spectrometry(GC-MS). The method can realizeonline connections of gel permeation chromatography, solid phase extraction and gas chromatography/mass spectrometry, eliminating themulti-step processmanually. Use ofgel columnincreasedthe sample injection volume to 200 μL, and sample loadwas 10 times than conventional micro silica gel column. Large volume fractions from liquid chromatography on line solid phase extraction can inject into gas chromatography, and improve the sensitivity effectively.The linear correlation coefficient was 0.9992 in 0.08- 10 ng/m Lrange of concentrations, the intra-dayrelative standard deviation(RSD) was 3.26%,the inter-dayrelative standard deviation(RSD) was 3.87%, the limit of detection(LOD) was 0.022 ng/L, the limit of quantification(LOQ) was 0.093 ng/L, and the recoveries ranged from 95.6% to 97.2% at three spiked levels.The method was proved to be automated, simple, fast,sensitiveand accurate,and suitable for determination of B[a]P in smoker urine samples.
A new method for the determination of benzo[a]pyrene(B[a]P) in smoker urine sampleswas developed by online gel permeation chromatography-solid phase extraction-gas chromatography/mass spectrometry(GPC-SPE-GC/MS) hyphenated system. Smoker urine samples were extracted with cyclohexane containing D12-B[a]P as internal standard. Then, the extract was separated by gel permeation chromatography, and B[a]Pfraction was cutting into thesolid phase extraction cartridge and was enriched. The enriched B[a]P was eluted by acetone, then was determined by gas chromatography- mass spectrometry(GC-MS). The method can realizeonline connections of gel permeation chromatography, solid phase extraction and gas chromatography/mass spectrometry, eliminating themulti-step processmanually. Use ofgel columnincreasedthe sample injection volume to 200 μL, and sample loadwas 10 times than conventional micro silica gel column. Large volume fractions from liquid chromatography on line solid phase extraction can inject into gas chromatography, and improve the sensitivity effectively.The linear correlation coefficient was 0.9992 in 0.08- 10 ng/m Lrange of concentrations, the intra-dayrelative standard deviation(RSD) was 3.26%,the inter-dayrelative standard deviation(RSD) was 3.87%, the limit of detection(LOD) was 0.022 ng/L, the limit of quantification(LOQ) was 0.093 ng/L, and the recoveries ranged from 95.6% to 97.2% at three spiked levels.The method was proved to be automated, simple, fast,sensitiveand accurate,and suitable for determination of B[a]P in smoker urine samples.
引文
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16 Purcaro G,Moret S,Conte L.Journal of Chromatography A,2012,1255,100-111
17 Luo Yan-Bo,Zheng Hao-Bo,Jiang Xing-Yi,Li Xue,Zhang Hong-Fei,Zhu Feng-Peng,Pang Yong-Qiang,Feng Yu-Qi.Chinese J.Anal.Chem.,2015,43(10):1538-1544
18 Liu Chun-Bo,Shen Qin-Peng,Zhang Feng-Mei,Zhang An-Feng,He Pei,Si Xiao-Xi,Liu Zhi-Hua,Yang Guang-Yu,Miao Ming-Ming.Chinese Journal ofanalytical chemistry,2016,44(2):241-246
2 LIU Jian-Fu,YU Xi,LIU De-Hua.Chinese Journal of Chromatography,2002,20(2):187-189
3 DU Xue-Qing,WANG Xin-Ming,TANG Jian-Hui.Environmental Chemistry,2006,25(6):785-788
4 Liu H C,Shao J L,Lin T,Li Q W.Chromatographia,2013,76(23-24):1785-1789
5 Wu Ping-Yan,Duan Meng,Guo Ting-Ting,Zhang Shi-Dong,Li Han.Chinese Journal of Spectroscopy Laboratory,2012,29(5):2984-2987
6 SHI Jia-Xin,LIU Bai-Zhan,XIE Wen-Yan.Chinese Journal of Chromatography,2010,28(6):623-627
7 Wang X Y,Wang Y,Qin Y Q,Li D,Chen Y,Xie F W.Talanta,2015,140:102-108
8 ZHANG Xia,LIU Zhi-Hua,KONG Wei-Song.Chinese Journal of Analysis Laboratory,2013,10:100-102
9 Jung K H,Noh J H,Eun J W,Kim J K,Bae H J,Xie H,Jang J J,Ryu J C,Park W S,Lee J Y,Environmental science&technology,2010,45,300~306
10 Peng F,Xue H H,Chen W C,Li Z Q.Advanced Materials Research.2015,1073:575-578
11 He W L,Hu X J,Li Z H,Chen X S,Liu M S.Asian Journal of Chemistry,2013,25(16):9216.
12 Ghasemzadeh-Mohammadi V,Mohammadi A,Hashemi M,Khaksar R,Haratian P.Journal of Chromatography A,2012,1237:30-36
13 Sanagi M M,Loh S H,Ibrahim W A W,Hasan M N,Aboul-Enein H Y.Journal of chromatographic science,2013,51(2):112-116
14 Kuosmanen K,Hy?tyl?inen T,Hartonen K,Riekkola M L.Journal of Chromatography A,2002,943(1):113-122.
15 Hy?tyl?inen T,Riekkola M L.Analytical and bioanalytical chemistry,2004,378(8),1936-1938
16 Purcaro G,Moret S,Conte L.Journal of Chromatography A,2012,1255,100-111
17 Luo Yan-Bo,Zheng Hao-Bo,Jiang Xing-Yi,Li Xue,Zhang Hong-Fei,Zhu Feng-Peng,Pang Yong-Qiang,Feng Yu-Qi.Chinese J.Anal.Chem.,2015,43(10):1538-1544
18 Liu Chun-Bo,Shen Qin-Peng,Zhang Feng-Mei,Zhang An-Feng,He Pei,Si Xiao-Xi,Liu Zhi-Hua,Yang Guang-Yu,Miao Ming-Ming.Chinese Journal ofanalytical chemistry,2016,44(2):241-246
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