圆盘膜萃取-气相色谱-质谱法同时测定水中16种酞酸酯类化合物
GC-MS Determination of 16 Phthalate Esters in Water by Disc Membrane Extraction
摘 要
提出了气相色谱-质谱法同时测定水中16种酞酸酯类化合物(PAEs)的方法。采用自制圆盘萃取装置、无塑料制品接触试验程序进行水样富集,对圆盘膜片选择、过膜压力、洗脱剂种类与用量等进行考察;对仪器工作条件离子源温度、升温速率、进样口温度和不同时间段监测离子及增益等进行了探讨。16种PAEs的质量浓度分别在一定的范围内与峰面积呈线性关系,检出限(3S/N)在0.17~2.45 μg·L-1之间。以空白蒸馏水为基底,在3个浓度水平下做加标回收试验,回收率在79.8%~104%之间,相对标准偏差(n=6)在1.1%~9.4%之间。
气相色谱-质谱法
酞酸酯
水
Disc membrane extraction
GC-MS
Phthalate esters
Water
Abstract
A method of GC-MS for the determination of 16 phthalate esters (PAEs) in water was proposed. Water sample was enriched by self-made disc extraction device with no plastic-contacting experimental procedures. Experimental conditions, including the choice of disc membrane, pressure of membrane, kind and amount of eluent, were studied; and the working condition of the instrument, including the temperature of ion source, rate of temperature elevation, temperature at the inlet of sample injection, monitoring ions and gains at different time intervals, were discussed. Under the optimum conditions, linear relationships between values of peak area and mass concentration of the 16 PAEs were obtained in definite ranges, with detection limits (3S/N) in the range of 0.17-2.45 μg·L-1. Test for recovery was made by addition of standards of the 16 PAEs at 3 different concentration levels to blank water samples as matrixes, values of recovery found were in the range of 79.8% to 104%, with RSD′s (n=6) in the range of 1.1%-9.4%.
中图分类号 O657.63
所属栏目 工作简报
基金项目 国家环境保护部公益项目(200909054);江苏省优势学科建设项目资助(苏政办发［2011］6号)
收稿日期 2011/12/19
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备注王丽(1984-),女,江苏镇江人,硕士研究生,主要从事食品安全研究。
引用该论文: WANG Li,LI Lei,ZHOU Jing-ping,XU Qiu-jin. GC-MS Determination of 16 Phthalate Esters in Water by Disc Membrane Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2012, 48(5): 570～575
王丽,李磊,周靖平,许秋瑾. 圆盘膜萃取-气相色谱-质谱法同时测定水中16种酞酸酯类化合物[J]. 理化检验－化学分册, 2012, 48(5): 570～575
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参考文献
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【2】PANT N, PANT A, SHUKLA M, et al. Environmental and experimental exposure of phthalate esters: the toxicological consequence on human sperm［J］. Hum Exp Toxicol, 2011,30:507-14.
【3】GUO Ying, WU Qian, KANNAN K. Phthalate metabolites in urine from China, and implications for human exposures［J］. Environ Int, 2011,37:893-898.
【4】FROMME H, GRUBER L, SECKIN E, et al. Phthalates and their metabolites in breast milk-results from the bavarian monitoring of breast milk (BAMBI)［J］. Environment International, 2011,37:715-722.
【5】GUO Ying, ALOMIRAH H, CHO H S, et al. Occurrence of phthalate metabolites in human urine from several asian countries［J］. Environmental Science and Technology, 2011,45:3138-3144.
【6】HE Huan, HU Guan-jiu, SUN Cheng, et al. Trace analysis of persistent toxic substances in the main stream of Jiangsu section of the Yangtze River, China［J］. Environmental Science and Pollution Research, 2011,18(4):638-648.
【7】SHI Wei, WANG Xiao-yi, HU Guan-jiu, et al. Bioanalytical and instrumental analysis of thyroid hormone disrupting compounds in water sources along the Yangtze River［J］. Environ Pollut, 2011,159:441-448.
【8】SIRIVITHAYAPAKORN S, THUYVIANG K. Dispersion and ecological risk assessment of di (2-ethylhexyl) phthalate (DEHP) in the surface waters of Thailand［J］. Bull Environ Contam Toxicol, 2010,84:503-506.
【9】ZENG Feng, WEN Jia-xin, CUI Kun-yuan, et al. Seasonal distribution of phthalate esters in surface water of the urban lakes in the subtropical city, Guangzhou, China［J］. Journal of Hazardous Materials, 2009,169(1/3):719-725.
【10】WANG Fan, XIA Xing-hui, SHA Yu-juan. Distribution of phthalic acid esters in Wuhan section of the yangtze river, china［J］. Journal of Hazardous Materials, 2008,154(1/3):317-324.
【11】ZENG Feng, CUI Kun-yuan, XIE Zhi-yong, et al. Occurrence of phthalate esters in water and sediment of urban lakes in a subtropical city, Guangzhou, South China［J］. Environment International, 2008,34(3):372-380.
【12】SHA Yu-juan, XIA Xing-hui, YANG Zhi-feng, et al. Distribution of PAEs in the middle and lower reaches of the Yellow River, China［J］. Environmental Monitoring and Assessment, 2007,124(1/3):277-287.
【13】王鑫,许小苗,俞晔.固相萃取-气相色谱法同时测定水中的酞酸酯类环境激素［J］.食品工业科技, 2008,29(4):287-289.
【14】王磊,张睿,程爱华,等.固相萃取气质联用测定水中邻苯二甲酸酯类物质［J］.中国给水排水, 2007,23(14):86-89.
【15】马继平,李茉,赵秀华,等.固相萃取-反相高效液相色谱法测定水中的邻苯二甲酸酯［J］.分析试验室, 2009,28(3):6-9.
【16】吴慧勤,朱志鑫,黄小兰,等.不同类别食品中21种邻苯二甲酸酯的气相色谱-质谱测定及其分布情况研究［J］.分析测试学报, 2011,30(10):1078-1087.
【17】梁颖,刘慧,王程,等.固相萃取-气相色谱法测定地下水中痕量酞酸酯的研究［J］.分析科学学报, 2009,25(3):333-336.
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