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  

Determination of tetracyclines in water using polythiophenes extraction and UV&HPLC

作　　者：王怡梅 江维 李漂洋 胡晓荣[1] WANG Yimei;JIANG Wei;LI Piaoyang;HU Xiaorong(College of Materials and Chemistry&Chemical Engineering,Chengdu University of Technology,Chengdu 610059,China)

机构地区：[1]成都理工大学材料与化学化工学院,四川成都610059

出　　处：《中国测试》2020年第8期63-69,共7页China Measurement & Test

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(V∶V=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 1.0μg/L。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 extractionhigh 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 0.0001-0.0005 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 1.0μg/L.

关 键 词：聚噻吩 四环素类 固相萃取 养殖水 

分 类 号：O657.7[理学—分析化学]