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首页> 《中国测试》期刊 >本期导读>聚噻吩萃取光度法和高效液相色谱法测定水体中四环素类的含量

聚噻吩萃取光度法和高效液相色谱法测定水体中四环素类的含量

184    2020-08-19

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作者:王怡梅, 江维, 李漂洋, 胡晓荣

作者单位:成都理工大学材料与化学化工学院,四川 成都 610059


关键词:聚噻吩;四环素类;固相萃取;养殖水


摘要:

以聚噻吩为萃取材料,优化对四环素类(TCs)抗生素的萃取条件,建立固相萃取-分光光度法(SPE-UV)、固相萃取-高效液相色谱法(SPE-HPLC)检测水体中TCs(OTC、TC、DOX)的分析方法。100 mL水样,调整pH=5.0,经50 mg聚噻吩萃取柱富集净化,甲醇/乙酸(VV=9∶1)解吸。SPE-UV法总量测定线性范围为0.15~2.4 mg/L,相关系数大于0.99;相对标准偏差为1.1%~4.5%(n=5);检出限为0.002 mg/L;对于100 mL 0.10 mg/L的TC和总量0.30 mg/L TCs标准溶液,萃取率分别为85%和70%;实际水样加标回收率99.7%~104%。SPE-HPLC法线性范围为0.005~1 mg/L,相关系数大于0.99;相对标准偏差为1.8%~3.0%(n=5);检出限为0.0001~0.0005 mg/L;对于100 mL 0.010 mg/L的OTC、TC、DOX标准溶液,萃取率分别为74%、94%、58%;实际水样加标回收率98.8%~115%。应用两种方法对三种水样进行检测,仅由SPE-HPLC检出鱼塘水中含TC 1.0 μg/L。


Determination of tetracyclines in water using polythiophenes extraction and UV&HPLC
WANG Yimei, JIANG Wei, LI Piaoyang, HU Xiaorong
College of Materials and Chemistry & Chemical Engineering, Chengdu University of Technology, Chengdu 610059, China
Abstract: Using polythiophenes as the extraction material and optimizing extraction conditions for tetracyclines (TCs), a solid phase extraction-spectrophotometric(SPE-UV) method and a solid phase extraction-high performance liquid chromatography (SPE-HPLC) method were developed for the determination of TCs (OTC, TC, DOX) in water. The 100 mL water samples, adjusting the acidity to pH=5.0, were enriched and purified by 50 mg polythiophenes column and desorbed by methanol/acetic acid (V:V=9:1). SPE-UV method was used to measure the total TCs with linear range of 0.15-2.4 mg/L. The correlation coefficient was not less than 0.99.The relative standard deviationwas 1.1%-4.5% (n=5). The detection limits was 0.002 mg/L. For 100 mL of 0.10 mg/L TC and 0.30 mg/L total TCs standard solution, the extraction rates were 85% and 70%, respectively. The recoveries of standard in actual water were 99.7%-104%. The linear range of SPE-HPLC were 0.005-1 mg/L with the correlation coefficient not less than 0.99. The relative standard deviation were 1.8%-3.0% (n=5). The detection limit were 0.000 1-0.000 5 mg/L. For 100 mL of 0.010 mg/L OTC, TC, DOX standard solution, the extraction rates were 74%, 94% and 58%, respectively. The recoveries of standard in actual water were 98.8%-115%. Three kinds of water samples were tested by two methods, and only TC was determined by SPE-HPLC in fish pond water with concentrations of 1.0 μg/L.

Keywords: polythiophenes;tetracyclines;solid phase extraction;aquaculture water
2020, 46(8):63-69  收稿日期: 2020-06-30;收到修改稿日期: 2020-07-25
基金项目:
作者简介: 王怡梅(1995-),女,四川资阳市人,硕士研究生,专业方向为分析化学
参考文献
[1] ADDISON J B. Antibiotics in sediments and run-off waters from feedlots[J]. Residue Reviews, 1984, 92: 1-28
[2] 陈青海. 水产养殖业中抗生素使用的风险及其控制[J]. 水产科技情报, 2009, 36(2): 56-59
[3] POMATI F, NETTING A G, CALAMARI D, et al. Effect of erythromycin, tetracycline and ibuprofen on the growth of Synechocystissp and Lemna minor[J]. Aquatic Toxicology, 2004, 67(4): 387-396
[4] SULTAN S M, ALZAMIL I Z, ALARFAJ N A. Complexometric-spectrophotometric assay of tetracyclines in drug formulations[J]. Talanta, 1988, 35(5): 375-378
[5] EMARA K M, HASSAN F, SALEH G A. Spectrophotometric determination of tetracycline an oxytetracycline in pharmaceutical preparations[J]. Talanta, 1991, 38(11): 1219-1222
[6] 胡献刚, 罗义, 周启星. 固相萃取-高效液相色谱法测定畜牧粪便中13种抗生素药物残留[J]. 分析化学, 2008, 36(9): 1162-1166
[7] 曾国龙, 马晓国, 樊银明. 多模板分子印迹聚合物磁性固相萃取-高效液相色谱法测定环境水样中四环素类抗生素[J]. 分析测试学报, 2020, 39(6): 749-755
[8] 程家兴, 赵起越, 李令军, 等. 固相萃取/超高效液相色谱-质谱法筛查及检测养鱼河水中抗生素[J]. 分析测试学报, 2018, 37(3): 275-281
[9] 杨旭, 刘美娇, 林深, 等. 限进材料固相萃取-高效液相色谱在线联用检测牛奶中四环素类抗生素残留[J]. 分析化学, 2016, 44(1): 146-151.
[10] LUO Y, LI B, WANG W, et al. Hypercrosslinked aromatic heterocyclic microporous polymers: a new class of highly selective CO2 capturing materials[J]. Advanced Materials, 2012, 24(42): 5703-5707
[11] CHEN J, ZHANG L, ZHU J, et al. Adsorption of polythiophene/TiO2 composite for Zn(II), Pb (II) and Cu (II): Selectivity and synergistic effect investigation[J]. Applied Surface Science, 2018, 459: 318-326
[12] KALYANI R, GURUNATHAN K. Metal ions doped and polythiophene coated nanophotocatalysts: Synthesis and spectroscopic characterization for H2 production and dye degradation[J]. Optik - International Journal for Light and Electron Optics, 2016: 4741-4745.
[13] FEIZBAKHSH A, EHTESHAMI S. Polythiophene–chitosan magnetic nanocomposite as a novel sorbent for disperse magnetic solid phase extraction of triazine herbicides in aquatic media[J]. Chromatographia, 2016, 79(17/18): 1177-1185.
[14] BAHARIN S N A, SARIH N M, MOHAMAD S, et al. Removal of endocrine disruptor di-(2-ethylhexyl) phthalate by modified polythiophene-coated magnetic nanoparticles: characterization, adsorption isotherm, kinetic study, thermodynamics[J]. RSC Advances, 2016, 6(50): 44655-44667.