Determination of Dieldrin and Polychlorinated Biphenyls in Seawater by Solid Phase Extraction and Capillary Gas Chromatography
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摘要: 狄氏剂与多氯联苯均是海洋环境中毒性大、难降解的有机污染物，建立海水中狄氏剂与多氯联苯快速、灵敏、准确的检测方法，具有重要意义。本文采用聚苯乙烯/二乙烯基苯(Cleanert PS)固相萃取柱对海水样品中的狄氏剂与7种多氯联苯进行分离富集,建立了气相色谱-电子捕获检测器(GC-μECD)的分析方法。实验了萃取流速、洗脱液、水样盐度与pH等实验条件对萃取效率的影响，确定样品以5.0 mL/min的流速经Cleanert PS固相萃取柱富集，真空抽干后用5.0 mL丙酮洗脱，挥干洗脱液，用1.0 mL正己烷定容，在选定的色谱条件下进行分析。方法精密度(RSD)为0.9%~4.4%，与《海洋监测规范》GB 17378.4—2007的RSD指标相比，精密度良好；加标回收率为82.1%~123.9%。狄氏剂的检出限(0.0088 μg/L)低于文献的检出限(0.05 μg/L)，7种多氯联苯的检出限(0.0012～0.0067 μg/L)低于文献的检出限(0.147～0.289 μg/L)。该方法适合于海水中痕量狄氏剂与多氯联苯的快速分析，具有一定的实用价值。Abstract: Dieldrin and polychlorinated biphenyls (PCBs) are toxic, organic pollutants that break down extremely slowly in the marine environment. Therefore, it is of valuable significance to establish a rapid, sensitive and accurate detection method for dieldrin and PCBs in seawater. A method has been developed for determining dieldrin and seven PCBs in seawater by Cleanert PS solid-phase extraction and capillary Gas Chromatography with an Electron Capture Detector (GC-μECD). Determination parameters, such as extracting flow rate, eluent, seawater salinity and pH and their effects for extraction efficiency are discussed. By the new method, dieldrin and seven PCBs were extracted from seawater under a flow rate of 5.0 mL/min, eluted by 5.0 mL acetone. The eluate was evaporated, and the solvent was set to 1.0 mL with hexane. The target compounds were determined by GC-μECD. The average recoveries of the method ranged from 82.1% to 123.9% with relative standard deviation (RSD) of 0.9%-4.4%. This method has a better precision compared with the RSD index (1.7%-7.7%) in the specification for marine monitoring (GB 17378.4—2007). The detection limit of dieldrin (0.0088 μg/L) is below the documentary detection limit (0.05 μg/L). Meanwhile, the detection limits of 7 kinds of PCBs range from 0.0012 to 0.0067 μg/L which are below their documentary detection limits (0.147-0.289 μg/L). The established method was qualified for rapid determination of dieldrin and PCBs in seawater samples with a good practical value.
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Key words:
- seawater /
- dieldrin /
- polychlorinated biphenyls /
- solid phase extraction /
- Gas Chromatography
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表 1 方法的线性方程、精密度和检出限
Table 1. The regression equations, RSDs and detection limits
化合物
(按保留时间的
先后顺序排列)线性方程 相关
系数RSD
(%)检出限
(μg/L)PCB 28 y=396.6x-21.3 0.9995 2.1 0.0012 PCB 52 y=380.8x-39.9 0.9994 3.3 0.0023 PCB 101 y=527.9x-5.1 0.9996 2.4 0.0067 狄氏剂 y=292.3x+2.9 0.9995 4.4 0.0088 PCB 118 y=455.6x+2.1 0.9999 2.1 0.0013 PCB 153 y=618.9x-17.8 0.9990 1.8 0.0028 PCB 138 y=552.8x-13.8 0.9994 0.9 0.0039 PCB 180 y=654.4x-4.6 0.9993 3.4 0.0019 
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表 2 样品测定与加标回收率
Table 2. Analytical results of real sample and spiked recovery
化合物 样品测定值
(μg/L)平均加标回收率(%) 水平1 水平2 水平3 PCB 28 0.56 108.1 100.6 99.2 PCB 52 1.37 102.9 106.5 119.0 PCB 101 0.54 105.4 103.9 90.8 狄氏剂 1.12 91.3 107.8 99.0 PCB 118 0.38 109.4 101.1 98.9 PCB 153 0.33 99.1 123.9 100.3 PCB 138 0.30 82.1 85.4 100.2 PCB 180 0.24 89.1 110.9 104.6
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[1] EP UN.Stockholm Convention on Persistent Organic Pollutants[R].UNEP/POPS/POPRC.4/INF/9, 2001.
[2] 罗慧,王新红,汤丽,洪丽玉,吴水平,谢卫.中国部分沿海海域水体中溶解态有机氯农药和多氯联苯的残留分布特征[J].海洋环境科学,2010,29(1):115-120. http://www.cnki.com.cn/Article/CJFDTOTAL-HYHJ201001027.htm
[3] Perez E, Len L, Parra G, Gonzelez E.Simultaneous de-terminati on of pesticides, polycyclic aromatic hydro-carbons and polychlorinated biphenyls in seawater and interstitial marine water samples, using stir bar sorptive extraction-thermal desorption-gas chromatography-mass spectrometry[J].Journal of Chromatography A,2009,1170(1/2):1551-1562.
[4] Loganathan G, Kannan K, Globa L.Organochlorine con-tamination trends: An overview[J].AMBIO,1994, 23(3):187-191.
[5] GB 17378.4-2007,海洋监测规范[S].2007: 47-57.
[6] EPA Method 8082A,Polychlorinated Biphenyls by Gas Chromatography[S].
[7] 魏爱泓,樊祥科,袁广旺,方南娟.毛细管柱气相色谱法测定海水中的多氯联苯[J].海洋环境科学,2007,26(6):580-582. http://www.cnki.com.cn/Article/CJFDTOTAL-HYHJ200706021.htm
[8] 王娜.液-液萃取富集-气相色谱法测定水中有机氯农药和多氯联苯[J].理化检验(化学分册),2011,47(3):327-330. http://www.cnki.com.cn/Article/CJFDTOTAL-LHJH201103028.htm
[9] 杨丽莉,母应锋,胡恩宇,王丽媛.固相萃取-GC/MS法测定水中有机氯农药[J].环境监测管理与技术,2008, 20(1):25-28. http://www.cnki.com.cn/Article/CJFDTOTAL-GSJU201502016.htm
[10] Chen F, Chen L, Wang Q, Zhou J, Xue X, Zhao J.Determination of organochlorine pesticides in propolis by gas chromatography-electron capture detection using double column series solid-phase extraction[J]. Analytical and Bioanalytical Chemistry, 2009, 393:1073-1079. doi: 10.1007/s00216-008-2474-1
[11] 邓敏军,罗艳,邓超冰.固相萃取-气相色谱-质谱法测定水中的19种多氯联苯[J].光谱实验室,2012,29(2):947-950. http://www.cnki.com.cn/Article/CJFDTOTAL-GPSS201202070.htm
[12] 邰超,齐永安,庞玉娟,赵同谦.固相微萃取-气相色谱法测定水中痕量有机氯农药[J].环境监测管理与技术, 2007,19(5):26-29. http://www.cnki.com.cn/Article/CJFDTOTAL-HJJS200705009.htm
[13] Ozcan S, Tor A, Aydin M E.Application of ultrasound-assisted emulsification-micro-extraction for the analysis of organochlorine pesticides in waters[J].Water Research, 2009, 43:4269-4277. doi: 10.1016/j.watres.2009.06.024
[14] 胡恩宇,杨丽莉,王美飞,母应锋.气相色谱法同时测定水中28种多氯联苯单体[J].环境监测管理与技术, 2010, 22(1):44-48. http://www.cnki.com.cn/Article/CJFDTOTAL-HJJS201001014.htm
[15] Wang S, Russo T, Qiao G, David H S, Robert A S.Admicellar polymerization of styrene with divinyl benzene on alumina particles: The synthesis of white reinforcing fillers[J]. Journal of Materials Science, 2006, 41:7474-7482. doi: 10.1007/s10853-006-0788-y
[16] 龙庆云,张洪彬,韦桂欢,李杰,闫云.固相萃取-气质联用测定水中半挥发性有机物研究[J].舰船科学技术,2010,32(12):102-106. doi: 10.3404/j.issn.1672-7649.2010.12.026
[17] 阎正,封棣,李申杰,赵亚奎,杨慧.固相萃取-毛细管气相色谱法测定中草药中13种有机氯农药的残留量[J].色谱,2005,23(3):308-311. http://www.cnki.com.cn/Article/CJFDTOTAL-SPZZ200503026.htm
[18] 李庆玲,徐晓琴,黎先春,王小如.固相微萃取-气相色谱质谱联用测定海水和沉积物间隙水中的痕量多环芳烃[J].中国科学(化学),2006,36(3):202-210. http://www.cnki.com.cn/Article/CJFDTOTAL-JBXK200603003.htm
[19] 刘金巍,王磊,安彩秀,肖凡,查晓康,高希娟.固相萃取-气相色谱法测定饮用水中的多氯联苯[J].岩矿测试,2011,30(5):611-616. http://www.cnki.com.cn/Article/CJFDTOTAL-YKCS201105020.htm
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