Determination of 15 Aldehyde and Ketone Carbonyl Compounds in Environmental Solid Matrix by Liquid Chromatography with 2,4-Dinitrophenylhydrazine Derivatization and Solid Phase Extraction
摘 要
样品10.000 g中加入200 mL pH 5.0的乙酸-乙酸钠缓冲溶液,翻转振荡18 h,离心。取100 mL提取液,加入pH 3.0的柠檬酸-柠檬酸钠缓冲溶液4 mL,3.00 g·L-1 2,4-二硝基苯肼(DNPH)衍生溶液(介质为乙腈) 6 mL,于室温超声衍生30 min。将衍生后的提取液用C18固相萃取柱萃取,乙腈洗脱并定容至10 mL。萃取液采用液相色谱-二极管阵列检测器测定其中15种醛酮类羰基化合物的含量。15种醛酮类羰基化合物的质量浓度在30.0~1.50×103μg·L-1内与其对应的峰面积呈线性关系,检出限(3.143s)为0.016~0.045 mg·kg-1。按标准加入法进行回收试验,丙酮的回收率为39.6%~43.3%,其他醛酮类化合物的回收率为69.0%~99.4%,测定值的相对标准偏差(n=6)为5.7%~18%。
Abstract
Acetic acid-sodium acetate buffer solution (pH 5.0, 200 mL) was added to 10.000 g of the sample, and the mixture was oscillated for 18 h and then centrifuged. The extract of 100 mL was taken and citric acid-sodium citrate buffer solution (pH 3.0, 4 mL) and 3.00 g·L-1 of 2,4-dinitrophenylhydrazine (DNPH) derivatized solution (acetonitrile as solvent, 6 mL) were added, and then the mixture was derivatized ultrasonically at room temperature for 30 min. The derivatives were further extracted by C18 solid phase extraction column, eluted with acetonitrile, and the eluant was diluted to 10 mL with acetonitrile. The 15 aldehyde and ketone carbonyl compounds were determined by liquid chromatography with diode array detector. Linear relationships between values of peak area and mass concentration of 15 aldehyde and ketone carbonyl compounds were found in the same range of 30.0-1.50×103μg·L-1, with detection limits ranging from 0.016 to 0.045 mg·kg-1. Tests for recovery were made by standard addition method, giving results in the range of 39.6%-43.3% for actone and 69.0%-99.4% for the other aldehydes and ketones, and RSDs (n=6) ranged from 5.7% to 18%.
中图分类号 O657.7 DOI 10.11973/lhjy-hx201807021
所属栏目 专题报道(环境分析)
基金项目 国家环境保护标准项目(2016-12)
收稿日期 2017/7/4
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备注李利荣,高级工程师,研究方向为环境有机污染物监测
引用该论文: LI Lirong,GUAN Yuchun,WU Yufeng,CUI Lianxi,ZHANG Zhaoyuan,WANG Xiaoguo,ZHAO Zhiqiang,WANG Yanli. Determination of 15 Aldehyde and Ketone Carbonyl Compounds in Environmental Solid Matrix by Liquid Chromatography with 2,4-Dinitrophenylhydrazine Derivatization and Solid Phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(7): 841~846
李利荣,关玉春,吴宇峰,崔连喜,张肇元,王效国,赵志强,王艳丽. 2,4-二硝基苯肼衍生-固相萃取-液相色谱法测定环境固体基质中15种醛酮类羰基化合物的含量[J]. 理化检验-化学分册, 2018, 54(7): 841~846
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参考文献
【1】王小波,李国强,孟建新.甲基橙-溴酸钾体系催化光度法测定微量甲醛[J].分析科学学报, 2004,20(3):335-336.
【2】祝惠英,郭素荣,石磊.毛细管气相色谱法测定空气中低分子醛酮化合物[J].青岛大学学报(工程技术版), 2002,17(1):90-92.
【3】王丽苹,任凤莲,吴名剑,等.固相萃取毛细管气相色谱法测定卷烟滤嘴中7种挥发性羰基化合物[J].分析试验室, 2009,28(2):116-119.
【4】SAKURAGAWA A, YONENO T, INOUE K, et al. Trace analysis of carbonyl compounds by liquid chromatography-mass spectrometry after collection as 2,4-dinitrophenylhydrazine derivatives[J]. Journal of Chromatography A, 1999,844(1/2):403-408.
【5】游金清,陈嘉彬,倪建彬,等.水分散直接衍生/高效液相色谱法测定烟用胶中的醛酮[J].中国胶黏剂, 2014,23(5):18-22.
【6】王伟,卢志刚,张桂珍.DNPH衍生化采样-溶剂解析-高效液相色谱法同时测定木制品中25种醛酮化合物[J].环境监控与预警, 2016,8(5):30-33.
【7】万小红,吴名剑,蒋新宇,等.直接衍生-离子液体富集-高效液相色谱法分析水基胶中脂肪族醛酮[J].色谱, 2011,29(12):1183-1187.
【8】邢俊波,曹红,张炯,等.柱前衍生化-高效液相色谱法同时测定含油脂药材中8种低分子羰基化合物[J].中国中医药信息杂志, 2013,20(12):46-48.
【9】霍茵,邱雄雄,詹松.超高效液相色谱测定空气中13种醛酮类化合物[J].环境化学, 2013,32(9):1823-1825.
【10】BVLDT A, LINDAHL R, LEVIN J O, et al. A diffusive sampling device for the determination of formaldehyde in air using N-methyl-4-hydrazino-7-nitrobenzofurazan (MNBDH) as reagent[J]. Journal of Environmental Monitoring Jem, 1999,1(1):39-43.
【11】KOBAYASHI K, TANAKA M, KAWAI S. Gas chromatographic determination of low-molecular-weight carbonyl compounds in aqueous solution as their O-(2,3,4,5,6-pentafluorobenzyl) oximes[J]. Journal of Chromatography A, 1980,187(2):413-417.
【12】MAGIN D F. Preparation and gas chromatographic characterization of benzyloximes and p-nitrobenzyloximes of short-chain (C1-C7) carbonyls[J]. Journal of Chromatography A, 1979,178(1):219-227.
【13】SWARIN S, LIPARI F. Determination of formaldehyde and other aldehydes by high performance liquid chromatography with fluorescence detection[J]. Journal of Liquid Chromatography, 2015,6(3):425-444.
【14】LEHMPUHL D W, BIRKS J W. New gas chromatographic-electron-capture detection method for the determination of atmospheric aldehydes and ketones based on cartridge sampling and derivatization with 2,4,6-trichlorophenylhydrazine[J]. Journal of Chromatography A, 1996,740(1):71-81.
【15】BVLDT A, KARST U. 1-Methyl-1-(2,4-dinitrophenyl)hydrazine as a new reagent for the HPLC determination of aldehydes[J]. Analytical Chemistry, 1997,69(17):3617-3622.
【16】BINDING N, KLÄNING H, KARST U, et al. Analytical reliability of carbonyl compound determination using 1,5-dansylhydrazine-derivatization[J]. Fresenius Journal of Analytical Chemistry, 1998,362(3):270-273.
【2】祝惠英,郭素荣,石磊.毛细管气相色谱法测定空气中低分子醛酮化合物[J].青岛大学学报(工程技术版), 2002,17(1):90-92.
【3】王丽苹,任凤莲,吴名剑,等.固相萃取毛细管气相色谱法测定卷烟滤嘴中7种挥发性羰基化合物[J].分析试验室, 2009,28(2):116-119.
【4】SAKURAGAWA A, YONENO T, INOUE K, et al. Trace analysis of carbonyl compounds by liquid chromatography-mass spectrometry after collection as 2,4-dinitrophenylhydrazine derivatives[J]. Journal of Chromatography A, 1999,844(1/2):403-408.
【5】游金清,陈嘉彬,倪建彬,等.水分散直接衍生/高效液相色谱法测定烟用胶中的醛酮[J].中国胶黏剂, 2014,23(5):18-22.
【6】王伟,卢志刚,张桂珍.DNPH衍生化采样-溶剂解析-高效液相色谱法同时测定木制品中25种醛酮化合物[J].环境监控与预警, 2016,8(5):30-33.
【7】万小红,吴名剑,蒋新宇,等.直接衍生-离子液体富集-高效液相色谱法分析水基胶中脂肪族醛酮[J].色谱, 2011,29(12):1183-1187.
【8】邢俊波,曹红,张炯,等.柱前衍生化-高效液相色谱法同时测定含油脂药材中8种低分子羰基化合物[J].中国中医药信息杂志, 2013,20(12):46-48.
【9】霍茵,邱雄雄,詹松.超高效液相色谱测定空气中13种醛酮类化合物[J].环境化学, 2013,32(9):1823-1825.
【10】BVLDT A, LINDAHL R, LEVIN J O, et al. A diffusive sampling device for the determination of formaldehyde in air using N-methyl-4-hydrazino-7-nitrobenzofurazan (MNBDH) as reagent[J]. Journal of Environmental Monitoring Jem, 1999,1(1):39-43.
【11】KOBAYASHI K, TANAKA M, KAWAI S. Gas chromatographic determination of low-molecular-weight carbonyl compounds in aqueous solution as their O-(2,3,4,5,6-pentafluorobenzyl) oximes[J]. Journal of Chromatography A, 1980,187(2):413-417.
【12】MAGIN D F. Preparation and gas chromatographic characterization of benzyloximes and p-nitrobenzyloximes of short-chain (C1-C7) carbonyls[J]. Journal of Chromatography A, 1979,178(1):219-227.
【13】SWARIN S, LIPARI F. Determination of formaldehyde and other aldehydes by high performance liquid chromatography with fluorescence detection[J]. Journal of Liquid Chromatography, 2015,6(3):425-444.
【14】LEHMPUHL D W, BIRKS J W. New gas chromatographic-electron-capture detection method for the determination of atmospheric aldehydes and ketones based on cartridge sampling and derivatization with 2,4,6-trichlorophenylhydrazine[J]. Journal of Chromatography A, 1996,740(1):71-81.
【15】BVLDT A, KARST U. 1-Methyl-1-(2,4-dinitrophenyl)hydrazine as a new reagent for the HPLC determination of aldehydes[J]. Analytical Chemistry, 1997,69(17):3617-3622.
【16】BINDING N, KLÄNING H, KARST U, et al. Analytical reliability of carbonyl compound determination using 1,5-dansylhydrazine-derivatization[J]. Fresenius Journal of Analytical Chemistry, 1998,362(3):270-273.
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