固相萃取-气相色谱法检测海水中邻苯二甲酸二丁酯
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摘要
建立了检测海水中的邻苯二甲酸二丁酯(DBP)的气相色谱分析方法。样品经玻璃纤维滤膜过滤,C_(18)固相萃取柱富集,乙酸乙酯洗脱,氮吹浓缩后1 mL甲醇溶解定容,气相色谱氢火焰离子化检测器测定,外标法定量。本实验对洗脱液处理过程、溶剂选择、上样方式和洗脱液用量这些影响萃取效率的条件进行了优化。DBP含量在6～240 ng/mL范围内线性关系良好,相关系数R> 0. 995,加标量为30～60 ng/mL范围回收率为89. 9%～109. 8%,相对标准偏差3. 8%～4. 1%。方法检出限5 ng/mL,定量限10 ng/mL。对东山湾的海水样品进行测定,测定结果与当地地理水文条件及人类活动具有一定相关性。该方法适用于大批量处理样品。
A gas chromatographic method for the determination of dibutyl phthalate( DBP) in seawater was established. The sample was filtered through a glass fiber filter,enriched on a C_(18) solid phase extraction column,eluted with ethyl acetate,concentrated by nitrogen blowing,and redissolved in1 m L of methanol. Then the obtained sample was measured by gas chromatography with a hydrogen flame ionization detector,and quantified by an external standard method. The eluent treatment process,solvent selection,sample loading method,and the amount of eluent were optimized,which might affect extraction efficiency. The linear relationship of DBP in the range of 6-240 ng/m L was good,the correlation coefficient R was greater than 0. 995,and the recoveries were between 89. 9%and 109. 8% with relative standard deviations of 3. 8% to 4. 1% in the spiked range of 30-60 ng/m L. The limit of detection of the method was 5 ng/m L and the limit of quantification was10 ng/m L. The method was applied to the determination of seawater samples in Dongshan Bay,Zhangzhou City,Fujian Province,and the results were correlated with the local geography and hydrological conditions. The method is suitable for large-scale processing of samples.
A gas chromatographic method for the determination of dibutyl phthalate( DBP) in seawater was established. The sample was filtered through a glass fiber filter,enriched on a C_(18) solid phase extraction column,eluted with ethyl acetate,concentrated by nitrogen blowing,and redissolved in1 m L of methanol. Then the obtained sample was measured by gas chromatography with a hydrogen flame ionization detector,and quantified by an external standard method. The eluent treatment process,solvent selection,sample loading method,and the amount of eluent were optimized,which might affect extraction efficiency. The linear relationship of DBP in the range of 6-240 ng/m L was good,the correlation coefficient R was greater than 0. 995,and the recoveries were between 89. 9%and 109. 8% with relative standard deviations of 3. 8% to 4. 1% in the spiked range of 30-60 ng/m L. The limit of detection of the method was 5 ng/m L and the limit of quantification was10 ng/m L. The method was applied to the determination of seawater samples in Dongshan Bay,Zhangzhou City,Fujian Province,and the results were correlated with the local geography and hydrological conditions. The method is suitable for large-scale processing of samples.
引文
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[2] Salazar Beltran D,Hinojosa Reyes L,Ruiz Ruiz E,Hernandez Ramirez A,Luis Guzman-Mar J. Talanta,2017,168:291
[3] Hu L,Shan W,Zhang Y,Li S,Gao H,Lu R,Zhang S,Zhou W. RSC. Adv.,2016,6(43):36223
[4] Amiri A,Chahkandi M,Targhoo A. Anal. Chim. Acta.,2017,950:64
[5] Leng G,Chen W,Wang Y. J. Sep. Sci.,2016,39(17):3392
[6] Li X,Yin P,Zhao L. Environ. Sci. Pollut. Res. Int.,2016,23(19):19341
[7] Farahani A,Ramezani M,Hassan J,Niazi A. J. Brazil. Chem. Soc.,2017,28(6):967
[8] Chen F. Fujian. Anal. Test,2014,23(3):33陈飞.福建分析测试,2014,23(3):33
[9] Zhang Z M,Zhang H H,Li J L,Yang G P. Chin. J. Anal. Chem.,2017,45(3):348
[10] Li J H,L L B. Strait. Pharm.,2016,28(1):45李建华,廖林波.海峡药学,2016,28(1):45
[11] Fernandez Gonzalez V,Moscoso Perez C,Muniategui Lorenzo S,Lopez Mahia P,Prada Rodriguez D. Talanta,2017,162:648
[12] Fernandez Amado M,Prieto Blanco M C,Lopez Mahia P,Muniategui Lorenzo S,Prada Rodriguez D. Chemosphere,2017,175:52
[13] Chao H C,Liao H W,Kuo C H. J. Chromatogr. A,2016,1445:149
[14] HY/T 179-2015,Determination of phthalates in Marine environment by gas chromatography mass spectrometry HY/T 179-2015,海洋环境中邻苯二甲酸脂类的测定气相色谱-质谱法
[15] Amiri A,Ghaemi F. Microchimica. Acta.,2017,184(10):3851
[16] Ma K P,Li Y,Wang D J,Ji W N. Occupation. Heal.,2015,31(13):1771马鲲鹏,李琰,王冬究,吉文宁.职业与健康,2015,31(13):1771
[17] Montevecchi G,Masino F,Zanasi L,Antonelli A. Food Chem.,2017,221:1354
[18] Zhao Q Y,Zhao H S,Liu B X. Chem. Eng. Equip.,2016,1(1):193赵起越,赵红帅,刘保献.化学工程与装备,2016,1(1):193