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Determination of trace tetracyclines in surface water by aluminum hydroxide coprecipitation coupled with high-performance liquid chromatography

机译:氢氧化铝共沉淀-高效液相色谱法测定地表水中痕量四环素

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摘要

A simple method for the determination of trace tetracyclines (TCs) in surface water samples by aluminum hydroxide coprecipitation coupled with high-performance liquid chromatography (HPLC) with UV detection was developed. Tetracyclines (oxytetracycline hydrochloride, tetracycline hydrochloride and chlortetracycline) were coprecipitated by aluminum hydroxide precipitate at pH 6,0. The obtained precipitate by centrifugation was dissolved with 1 mol L~(-1) HCI, and the pH of the solution was adjusted to 4.0 for HPLC analysis. The solution pH value, adsorption time for coprecipitation, centrifugation rate and time were optimized. Under the optimum conditions, calibration curves of the tetracyclines were in the range of 5-50 ng mL~(-1), with a relative coefficient (R2) of 0.9960 and a limit of detection (LOD) of 0.115 ng L~(-1) for chlortetracycline (CTC), of 0.9990 and 0.0935 ng L~(-1) for oxytetracycline (OTC), and 0.9990 and 0.0817 ng L~(-1) for tetracycline (TC). The proposed method was applied to river water and lake water samples, and the recoveries were in the range of 81.70% to 96.45%, at three spiked concentration levels of 15 ng mL~(-1), 30 ng mL~(-1) and 40 ng mL~(-1).
机译:建立了一种通过氢氧化铝共沉淀-高效液相色谱-紫外检测法测定地表水中痕量四环素的简单方法。四环素(盐酸土霉素,四环素盐酸盐和金霉素)通过氢氧化铝沉淀在pH 6.0下共沉淀。通过离心获得的沉淀物用1mol L〜(-1)HCl溶解,并将溶液的pH调节至4.0以进行HPLC分析。优化了溶液的pH值,共沉淀吸附时间,离心率和时间。在最佳条件下,四环素的校正曲线在5-50 ng mL〜(-1)范围内,相对系数(R2)为0.9960,检出限(LOD)为0.115 ng L〜(- 1)对于金霉素(CTC),对于土霉素(OTC)为0.9990和0.0935 ng L〜(-1),对于四环素(TC)为0.9990和0.0817 ng L〜(-1)。该方法用于河流水和湖水样品,三种浓度浓度分别为15 ng mL〜(-1),30 ng mL〜(-1)时,回收率在81.70%至96.45%之间。和40 ng mL〜(-1)。

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