超声提取-气相色谱-质谱法测定水体沉积物中16种多环芳烃
GC-MS Determination of 16 Polycyclic Aromatic Hydrocarbons in Water Sediment by Ultrasonic Extraction
摘 要
以二氯甲烷为提取剂对水体沉积物中16种多环芳烃进行提取,弗罗里硅土柱净化,所得净化液浓缩至约0.5 mL,用Rtx-5MS毛细管柱进行分离。采用质谱检测器根据NIST05谱图库比对进行定性分析;采用氢火焰离子化检测器按外标法进行气相色谱定量分析。结果表明:16种多环芳烃的检出限(3S/N)在0.27~6.0 μg·kg-1之间。用标准加入法测得回收率在56%~96%之间,相对标准偏差(n=5)在1.2%~8.3%之间。
气相色谱-氢火焰离子化检测法
多环芳烃
沉积物
GC-MS
GC-FID
Polycyclic aromatic hydrocarbons
Sediments
Abstract
Sixteen polycyclic aromatic hydrocarbons (PAH′s) were separated from water sediment by ultrasonic extraction with CH2Cl2, and the extract was purified and concentrated to about 0.5 mL. Rtx-5MS capillary column was used for separation. The identification of the 16 PAH′s was performed by comparing spectra obtained by MS detector with NIST05 atlas database; and quantification was performed by GC using external standard method with hydrogen flame ionization detector (FID). Values of detection limit (3S/N) of the method found were in the range of 0.27-6.0 μg·kg-1. Values of recovery found by the standard addition method, were ranged from 56% to 96% with RSD′s (n=5) ranged from 1.2% to 8.3%.
中图分类号 O657.63
所属栏目 工作简报
基金项目 吉林化工学院科技计划项目(0653-02)
收稿日期 2012/1/26
修改稿日期
网络出版日期
作者单位点击查看
备注谢莹(1981-),女,吉林人,讲师,硕士研究生,主要研究方向为环境微生物学。
引用该论文: XIE Ying,ZHANG Tao,WEI Wei,WANG Jian-gang. GC-MS Determination of 16 Polycyclic Aromatic Hydrocarbons in Water Sediment by Ultrasonic Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2013, 49(2): 211～215
谢莹,张涛,魏薇,王建刚. 超声提取-气相色谱-质谱法测定水体沉积物中16种多环芳烃[J]. 理化检验－化学分册, 2013, 49(2): 211～215
被引情况:
【1】陈月萌,赵敏,王千,童月婵,王金凤, "毛细管气相色谱法测定工作场所空气中3种多环芳烃",理化检验－化学分册 50, 1409-1411(2014)
【2】周韵,马明,周宇艳, "液液萃取-气相色谱-质谱法测定墨水中的16种多环芳烃",理化检验－化学分册 50, 1521-1525(2014)
【3】张智芳,高雯雯,陈碧, "气相色谱-质谱法测定兰炭废水中有机污染物",理化检验－化学分册 50, 122-125(2014)
【4】周韵,马明,周宇艳, "液液萃取-气相色谱-质谱法测定墨水中的16种多环芳烃",理化检验－化学分册 50, 1521-1525(2014)
共有人对该论文发表了看法，其中：
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
参考文献
【1】潘峰,王艺霏,郑松涛.超声-索氏提取法提取焦化厂土壤中多环芳烃［J］.河南师范大学学报:自然科学版, 2010,38(5):122-124.
【2】李海燕,李楠,于丹丹.微波萃取-气质联用测定土壤中的16种多环芳烃［J］.环境监控与预警, 2010(1):20-23.
【3】梁柱,余雯静,孙欣阳.加速溶剂萃取-色谱质谱联用法测定土壤中的多环芳烃［J］.化学分析计量, 2009(3):45-48.
【4】黄铁民,赵法,吴松恒,等.胶束体系中测定苯并(a)芘的荧光分光光度法II.环境水样中微量苯并(a)芘的测定［J］.中国环境监测, 1995,11(3):15-16.
【5】钱薇,倪进治,骆永明,等.高效液相色谱-荧光检测法测定土壤中的多环芳烃［J］.色谱, 2007,25(2):221-225.
【6】LI A, UCHIMURA T, TSUKATANI H, et al. Trace analysis of polycyclic aromatic hydrocarbons using gas chromatography-mass spectrometry based on nanosecond multiphoton ionization［J］. Analytical Sciences, 2010,26:841-846.
【7】邹辉,罗岳平,陈一清,等.加速溶剂萃取-气相色谱法测定土壤中16种多环芳烃［J］.分析试验室, 2008,27(S1):37-39.
【8】陈虹丽,薛秀玲.浊点萃取-高效液相色谱测定土壤及底泥中痕量多环芳烃［J］.环境化学, 2009,28(3):441-444.
【9】刘颖,陈玲,唐银健,等.高效液相色谱法测定黄浦江表层沉积物中的痕量多环芳烃［J］.色谱, 2007,25(3):356-361.
【10】周翔.快速溶剂萃取-SPE硅胶柱净化-高效液相色谱法测定土壤中多环芳烃16种化合物的研究［J］.河南化工, 2010,27(10):57-58.
【11】黄宏,黄长江,陈图锋,等.超声波萃取-高效液相色谱法在海洋沉积物样品多环芳烃分析中的运用［J］.海洋技术, 2006(1):67-72.
【12】黄东勤,王盛才,陈一清,等.加速溶剂萃取-高效液相色谱法测定土壤中16种多环芳烃［J］.中国环境监测, 2008,24(3):26-29.
【13】NIKOLAOU A, KOSTOPOULOU M, LOFRANO G, et al. Determination of PAHs in marine sediments: analytical methods and environmental concerns［J］. Global NEST Journal, 2009,11(4):391-405.
【14】ANYAKORA C, OGBECHE A, PALMER P, et al. GC/MS analysis of polynuclear aromatic hydrocarbons in sediment samples from the Niger Delta region［J］. Chemosphere, 2005,60(7):990-997.
【15】贺行良,夏宁,张媛媛,等.ASE/GC-MS法同时测定海洋沉积物中65种多氯联苯、多环芳烃与有机氯农药［J］.分析测试学报, 2011,30(2):152-160.
【16】LI Qing-ling, XU Xiao-qin, LEE F S C, et al. Determination of trace PAHs in seawater and sediment pore-water by solid-phase microextraction［J］. Science In China Series B (Chemistry), 2006,49(6):481-491.
【17】CAM D, GAGNI S, MELDOLESI L, et al. Determination of polycyclic aromatic hydrocarbons in sediment using solid-phase microextraction with gas chromatography-mass spectrometry［J］. J Chromatogr Sci, 2000,38(2):55-60.
【18】BOONYATUMANOND R, WATTAYAKORN G, TOGO A, et al. Distribution and origins of polycyclic aromatic hydrocarbons (PAHs) in riverine, estuarine, and marine sediments in Thailand［J］. Marine Pollution Bulletin, 2006,52(8):942-956.
【19】李庆玲,徐晓琴,黎先春,等.加速溶剂萃取/气相色谱-质谱测定海洋沉积物中的痕量多环芳烃［J］.分析测试学报, 2006,25(5):33-37.
【20】廖翀,杨坪,赵云芝,等.串联四极杆质谱(GC-QqQ-MS/MS)测定土壤中的邻苯二甲酸酯与多环芳烃［J］.中国环境监测, 2008,24(5):12-16.
【21】张晓梅,张竹青,黄文鹏.超声萃取-高效液相色谱法测定土壤中多环芳烃［J］.环境科学与管理, 2010,35(7):124-127.
【22】张利飞,黄业茹,史双昕,等.土壤中多环芳烃和酞酸酯类有机污染物气相色谱-质谱测定方法中的质量控制与质量保证［J］.色谱, 2010,28(5):465-469.
【23】张小辉,王晓雁.气相色谱-质谱联用法测定土壤中16种多环芳烃［J］.岩矿测试, 2010,29(5):535-538.
【24】林琳,王海,缪丽娜,等.微波提取高效液相色谱法测定土壤中15种痕量多环芳烃［J］.中国环境监测, 2009,25(2):86-89.
【25】FILIPKOWSKA A, LUBECKI L, KOWALEWSKA G. Polycyclic aromatic hydrocarbon analysis in different matrices of the marine environment［J］. Anal Chim Acta, 2005,547:243-254.
【26】KOSTOPOULOU M, MYLONA A, NIKOLAOU A, et al. The 10th international conference on environmental science and technology［C］. Kos Island: s.n., 2007:723-729.
【2】李海燕,李楠,于丹丹.微波萃取-气质联用测定土壤中的16种多环芳烃［J］.环境监控与预警, 2010(1):20-23.
【3】梁柱,余雯静,孙欣阳.加速溶剂萃取-色谱质谱联用法测定土壤中的多环芳烃［J］.化学分析计量, 2009(3):45-48.
【4】黄铁民,赵法,吴松恒,等.胶束体系中测定苯并(a)芘的荧光分光光度法II.环境水样中微量苯并(a)芘的测定［J］.中国环境监测, 1995,11(3):15-16.
【5】钱薇,倪进治,骆永明,等.高效液相色谱-荧光检测法测定土壤中的多环芳烃［J］.色谱, 2007,25(2):221-225.
【6】LI A, UCHIMURA T, TSUKATANI H, et al. Trace analysis of polycyclic aromatic hydrocarbons using gas chromatography-mass spectrometry based on nanosecond multiphoton ionization［J］. Analytical Sciences, 2010,26:841-846.
【7】邹辉,罗岳平,陈一清,等.加速溶剂萃取-气相色谱法测定土壤中16种多环芳烃［J］.分析试验室, 2008,27(S1):37-39.
【8】陈虹丽,薛秀玲.浊点萃取-高效液相色谱测定土壤及底泥中痕量多环芳烃［J］.环境化学, 2009,28(3):441-444.
【9】刘颖,陈玲,唐银健,等.高效液相色谱法测定黄浦江表层沉积物中的痕量多环芳烃［J］.色谱, 2007,25(3):356-361.
【10】周翔.快速溶剂萃取-SPE硅胶柱净化-高效液相色谱法测定土壤中多环芳烃16种化合物的研究［J］.河南化工, 2010,27(10):57-58.
【11】黄宏,黄长江,陈图锋,等.超声波萃取-高效液相色谱法在海洋沉积物样品多环芳烃分析中的运用［J］.海洋技术, 2006(1):67-72.
【12】黄东勤,王盛才,陈一清,等.加速溶剂萃取-高效液相色谱法测定土壤中16种多环芳烃［J］.中国环境监测, 2008,24(3):26-29.
【13】NIKOLAOU A, KOSTOPOULOU M, LOFRANO G, et al. Determination of PAHs in marine sediments: analytical methods and environmental concerns［J］. Global NEST Journal, 2009,11(4):391-405.
【14】ANYAKORA C, OGBECHE A, PALMER P, et al. GC/MS analysis of polynuclear aromatic hydrocarbons in sediment samples from the Niger Delta region［J］. Chemosphere, 2005,60(7):990-997.
【15】贺行良,夏宁,张媛媛,等.ASE/GC-MS法同时测定海洋沉积物中65种多氯联苯、多环芳烃与有机氯农药［J］.分析测试学报, 2011,30(2):152-160.
【16】LI Qing-ling, XU Xiao-qin, LEE F S C, et al. Determination of trace PAHs in seawater and sediment pore-water by solid-phase microextraction［J］. Science In China Series B (Chemistry), 2006,49(6):481-491.
【17】CAM D, GAGNI S, MELDOLESI L, et al. Determination of polycyclic aromatic hydrocarbons in sediment using solid-phase microextraction with gas chromatography-mass spectrometry［J］. J Chromatogr Sci, 2000,38(2):55-60.
【18】BOONYATUMANOND R, WATTAYAKORN G, TOGO A, et al. Distribution and origins of polycyclic aromatic hydrocarbons (PAHs) in riverine, estuarine, and marine sediments in Thailand［J］. Marine Pollution Bulletin, 2006,52(8):942-956.
【19】李庆玲,徐晓琴,黎先春,等.加速溶剂萃取/气相色谱-质谱测定海洋沉积物中的痕量多环芳烃［J］.分析测试学报, 2006,25(5):33-37.
【20】廖翀,杨坪,赵云芝,等.串联四极杆质谱(GC-QqQ-MS/MS)测定土壤中的邻苯二甲酸酯与多环芳烃［J］.中国环境监测, 2008,24(5):12-16.
【21】张晓梅,张竹青,黄文鹏.超声萃取-高效液相色谱法测定土壤中多环芳烃［J］.环境科学与管理, 2010,35(7):124-127.
【22】张利飞,黄业茹,史双昕,等.土壤中多环芳烃和酞酸酯类有机污染物气相色谱-质谱测定方法中的质量控制与质量保证［J］.色谱, 2010,28(5):465-469.
【23】张小辉,王晓雁.气相色谱-质谱联用法测定土壤中16种多环芳烃［J］.岩矿测试, 2010,29(5):535-538.
【24】林琳,王海,缪丽娜,等.微波提取高效液相色谱法测定土壤中15种痕量多环芳烃［J］.中国环境监测, 2009,25(2):86-89.
【25】FILIPKOWSKA A, LUBECKI L, KOWALEWSKA G. Polycyclic aromatic hydrocarbon analysis in different matrices of the marine environment［J］. Anal Chim Acta, 2005,547:243-254.
【26】KOSTOPOULOU M, MYLONA A, NIKOLAOU A, et al. The 10th international conference on environmental science and technology［C］. Kos Island: s.n., 2007:723-729.
相关信息
