分散液液微萃取-气相色谱-质谱法测定长江水体中18种苯系物
GC-MS Determination of 18 Benzene Homologs in Waters of Yangtze River with Separation by Dispersive Liquid-Liquid Microextraction
摘 要
取经滤膜过滤的长江水样8.00 mL,加入含四氯乙烯10 μL的丙酮0.50 mL,样品中的苯系物在几秒钟内即被萃取至四氯乙烯微小液滴中。经高速离心,萃取相沉积在离心管底部,移取萃取相8 μL置于进样瓶中供气相色谱-质谱分析。在气相色谱分离中用HP-INNOWAX毛细管柱为固定相,在质谱分析中采用全扫描和选择离子检测模式。18种苯系物的质量浓度在1 000 μg·L-1以内与其峰面积呈线性关系,方法的检出限(3S/N)在0.055~0.156 μg·L-1之间。加标回收率在66.5%~106%之间,相对标准偏差(n=5)在3.1%~8.6%之间。
苯系物
分散液-液微萃取
长江水体
GC-MS
Benzene homologs
Dispersive liquid-liquid microextraction
Waters of Yangtze river
Abstract
8.00 mL of the filtered river water sample was taken treated by DLLME with 0.50 mL of acetone (containing 10 μL of Cl2-C=C-Cl2), and the 18 benzene homologs were extracted into the micro-droplets of Cl2-C=C-Cl2 within a few seconds. After centrifugation at high-speed, the extract-phase was separated at the bottom of centrifuging tube. 8 μL of the extract-phase was taken and placed into the sample bottle for GC-MS analysis. The HP-INNOWAX capillary column was used for GC separation and the full-scanning mode as well as the selected ion monitoring mode was adopted in MS determination. Linear relationships between values of peak area and mass concentration of the 18 benzene homologs were kept in ranges within 1 000 μg·L-1. Detection limits(3S/N) found were ranged from 0.055 to 0.156 μg·L-1. Values of recovery found by standard addition method were in the range of 66.5%-106%, with RSD′s (n=5) in the range of 3.1%-8.6%.
中图分类号 O657.63
所属栏目 工作简报
基金项目 江苏检验检疫系统科研项目(2006KJ06;2007KJ07)
收稿日期 2013/7/28
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备注张爱平(1979-),男,江苏南通人,工程师,硕士,主要从事光谱、色谱、电化学等方面的检验和科研工作。
引用该论文: ZHANG Ai-ping,WANG Hong-wei,WENG Li-feng,HOU Jin,FANG Yu-zhi. GC-MS Determination of 18 Benzene Homologs in Waters of Yangtze River with Separation by Dispersive Liquid-Liquid Microextraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2014, 50(9): 1104～1108
张爱平,王红卫,翁利丰,侯晋,方禹之. 分散液液微萃取-气相色谱-质谱法测定长江水体中18种苯系物[J]. 理化检验－化学分册, 2014, 50(9): 1104～1108
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参考文献
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【15】FARINA L, BOIDO E, CARRAU F, et al. Determination of volatile phenols in red wine by dispersive liquid-liquid microextraction and gas chromatography-mass spectrometry detection［J］. J Chromatogr A, 2007,1157:46-50．
【16】LIANG Pei, XU Jing, LI Qian. Application of dispersive liquid-liquid microextraction and high-performance liquid chromatography for the determination of three phthalate esters in water sample［J］. Anal Chim Acta, 2008,609:53-58．
【17】FATTAHI N, ASSADI Y, HOSSEINI M R M, et al. Determination of chlorophenols in water samples using simultaneous dispersive liquid-liquid microextraction and derivatization followed by gas chromatography-electron-capture detection［J］. J Chromatogr A, 2007,1157:23-29．
【18】臧晓欢,王春,高书涛,等.分散液相微萃取-气相色谱联用分析水样中菊酯类农药残留［J］.分析化学, 2008,36(6):765-769．
【19】刁春鹏,赵汝松,柳仁民,等.分散液相微萃取-气相色谱/质谱快速分析水中的硝基苯类化合物［J］.分析试验室, 2009,28(6):9-12．
【20】张建华,黄颖,陈晓秋,等.分散液-液微萃取-高效液相色谱法测定环境水样中的多环芳烃［J］.色谱, 2009,27(6):799-803．
【21】祝本琼,陈浩,李胜清.基于轻质萃取剂的溶剂去乳化分散液-液微萃取-气相色谱法测定水样中多环芳烃［J］.色谱, 2012,30(2):201-206．
【22】张晓赟,张丽君,张占恩.分散液液微萃取-气相色谱/质谱法测定水中多环芳烃［J］.分析科学学报, 2012,28(2):192-196．
【23】李晓晶,陈安,黄聪,等.分散液液微萃取-气相色谱法快速测定水中23种有机磷农药［J］.分析测试学报, 2011,30(3):326-329．
【24】周欣,臧晓欢,王东跃,等.分散液相微萃取-气相色谱联用测定葡萄中百菌清、克菌丹和灭菌丹残留［J］.分析化学, 2009,37(1):41-45．
【2】李萡,李扬秋.苯致血液、免疫毒性及T细胞受体分析在接苯人群中的应用［J］.国外医学卫生学分册, 2007,34(3):144-148．
【3】李森华,杨爱初,谢圈强,等.苯及其同系物接触者血清神经特异性烯化酶及碱性蛋白水平变化［J］.中国职业医学, 2008,35(1):13-15．
【4】叶露,王永桔.二硫化碳萃取毛细管柱气相色谱法测定水质的苯系物［J］.污染防治技术, 2005,18(6):53-54．
【5】陈国怔,王炫征,钱洪智,等.正已烷萃取气相色谱法测定水中苯系物［J］.中国卫生检验杂志, 2006,16(4):491-492．
【6】王若苹,杨红斌.固相微萃取-毛细管气相色谱法快速分析水中苯系物［J］.现代科学仪器, 2002(3):45-47．
【7】贾金平,冯雪,方能虎,等.活性碳纤维固相微萃取/气相色谱-质谱联用测定水中苯系物［J］.色谱, 2002,20(1):63-65．
【8】陈斌生,陶晶,韩志宁,等.吹脱捕集-毛细管气相色谱法测定饮用水及水源水中苯系物［J］.中国卫生检验杂志, 2009,19(9):2008-2009．
【9】葛萍,韩鸿印,张俊刚,等.吹扫捕集-气相色谱法测定水中苯系物［J］.化学分析计量, 2005,14(2):32-33．
【10】华树岸,黄秋艳,李志涛.吹扫捕集-气相色谱-质谱联用测定城市饮用水中苯系物［J］.光谱实验室, 2005,22(3):641-644．
【11】金钰.捕集阱顶空-气相色谱法测定水中低浓度苯系物［J］.分析化学, 2008,36(11):1567-1570．
【12】韩康,周建科,张前莉,等.顶空单液滴微萃取-气相色谱法测定水中苯系物［J］.理化检验-化学分册, 2008,44(2):154-156．
【13】REZAEE M, ASSADI Y, HOSSEINI M R M, et al. Determination of organic compounds in water using dispersive liquid-liquid microextraciton［J］. J Chromatogr A, 2006,1116:1-9．
【14】BERIJANI S, ASSADI Y, ANBIA M, et al. Dispersive liquid-liquid microextraction combined with gas chromatography-flame photometric detection very simple, rapid and sensitive method for the determination of organophosphorus pesticides in water［J］. J Chromatogr A, 2006,1123:1-9．
【15】FARINA L, BOIDO E, CARRAU F, et al. Determination of volatile phenols in red wine by dispersive liquid-liquid microextraction and gas chromatography-mass spectrometry detection［J］. J Chromatogr A, 2007,1157:46-50．
【16】LIANG Pei, XU Jing, LI Qian. Application of dispersive liquid-liquid microextraction and high-performance liquid chromatography for the determination of three phthalate esters in water sample［J］. Anal Chim Acta, 2008,609:53-58．
【17】FATTAHI N, ASSADI Y, HOSSEINI M R M, et al. Determination of chlorophenols in water samples using simultaneous dispersive liquid-liquid microextraction and derivatization followed by gas chromatography-electron-capture detection［J］. J Chromatogr A, 2007,1157:23-29．
【18】臧晓欢,王春,高书涛,等.分散液相微萃取-气相色谱联用分析水样中菊酯类农药残留［J］.分析化学, 2008,36(6):765-769．
【19】刁春鹏,赵汝松,柳仁民,等.分散液相微萃取-气相色谱/质谱快速分析水中的硝基苯类化合物［J］.分析试验室, 2009,28(6):9-12．
【20】张建华,黄颖,陈晓秋,等.分散液-液微萃取-高效液相色谱法测定环境水样中的多环芳烃［J］.色谱, 2009,27(6):799-803．
【21】祝本琼,陈浩,李胜清.基于轻质萃取剂的溶剂去乳化分散液-液微萃取-气相色谱法测定水样中多环芳烃［J］.色谱, 2012,30(2):201-206．
【22】张晓赟,张丽君,张占恩.分散液液微萃取-气相色谱/质谱法测定水中多环芳烃［J］.分析科学学报, 2012,28(2):192-196．
【23】李晓晶,陈安,黄聪,等.分散液液微萃取-气相色谱法快速测定水中23种有机磷农药［J］.分析测试学报, 2011,30(3):326-329．
【24】周欣,臧晓欢,王东跃,等.分散液相微萃取-气相色谱联用测定葡萄中百菌清、克菌丹和灭菌丹残留［J］.分析化学, 2009,37(1):41-45．
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