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Abstract：
The abuse and irrational use of tetracyclines (TCs) in human medicine and animal husbandry has become a serious concern, affecting the ecological environment and human health. The aim of this study was to develop a sensitive and selective method using fully automatic solid-phase extraction coupled with ultra-performance liquid chromatography-tandem mass spectrometry for the determination of twelve TCs in water. Four isotope-labeled internal standards for TCs were used to correct matrix effects. Several parameters affecting extraction efficiency were systematically optimized, and the optimum experimental conditions found were 1.0 L water sample with 0.5 g/L Na2EDTA (pH 3.0) extracted and enriched by CNW HLB cartridge and eluted by 4 mL of acetone:methanol (v/v, 1:1). The enrichment factors were up to 798-1059 but only requiring about 60 min per six samples. Under the optimized conditions, the linearity of the method ranged from 0.2 to 100 μg/L for 12 TCs, the detection limits were as low as 0.01-0.15 ng/L, and the recoveries were in the range of 70%-118%, with relative standard deviations less than 15%. The developed method can be successfully utilized for the determination of 12 TCs in pure water, tap water, river water, and mariculture seawater. In summary, three and six TCs were detected in river water and mariculture seawater, respectively, with total concentrations of 0.074-0.520 ng/L (mean 0.248 ng/L) and 0.792-58.369 ng/L (12.629 ng/L), respectively. Tetracycline (TC) and oxytetracycline (OTC) were the dominant TCs in river water, while doxytetracycline (DXC) and OTC were dominant in mariculture seawater.
摘要：
四环素类药物(TCs)在人类医药和畜牧业中的滥用和不合理使用已成为一个严重的问题,影响生态环境和人类健康。本研究的目的是建立一种灵敏，选择性的全自动固相萃取-超高效液相色谱-串联质谱法测定水中12种TC的方法。使用四种同位素标记的TC内标来校正基体效应。对影响提取效率的几个参数进行了系统的优化,发现的最佳实验条件是1.0L水样，0.5g/LNa2EDTA（pH3.0），用CNWHLB柱提取和富集，用4mL丙酮：甲醇（v/v，1:1).富集因子高达798-1059，但每六个样品仅需要约60分钟。在优化条件下,对于12个TC，该方法的线性范围为0.2至100μg/L，检出限低至0.01-0.15ng/L，回收率在70%-118%之间,相对标准偏差小于15%。该方法可成功用于纯水中12种TCs的测定,自来水,河水,和海水养殖。总之,在河水和海水养殖海水中检测到三个和六个TC，分别,总浓度为0.074-0.520ng/L（平均0.248ng/L）和0.792-58.369ng/L（12.629ng/L），分别。四环素（TC）和土霉素（OTC）是河水中的主要TC，海水养殖海水中多西四环素（DXC）和OTC占优势。
