高效液相色谱法同时测定废水中扑热息痛和双氯芬酸的含量

N. Thanh, N. Dong, Thi Thu, Trang, N. Việt, Hoang Pham Tuan, Pham Thi Linh, Yen
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摘要

本研究建立了一种简便、选择性、准确的分析方法,用于同时测定废水处理系统中存在的消炎药(扑热息痛和双氯芬酸)的含量。该方法采用固相萃取法(SPE)和反相高效液相色谱法(HPLC-PDA)。采用HSR C18色谱柱(250 mm × 4.6 mm;5µm),流动相为乙腈:正磷酸二氢钠,比例为60:40 v/v。流速为1 ml/min,对乙酰氨基酚和双氯芬酸分别在243 nm和276 nm检测PDA。对乙酰氨基酚和双氯芬酸的持续时间分别为2.39 min和4.39 min。结果表明,所建立的方法在0.01 ~ 1µg/ml和0.02 ~ 1µg/ml范围内对扑热息痛和双氯芬酸的含量具有良好的准确度、精密度和线性关系。对乙酰氨基酚和双氯芬酸的检出限分别为0.003µg/ml和0.006µg/ml,定量限分别为0.01µg/ml和0.02µg/ml。对乙酰氨基酚和双氯芬酸的加样回收率均大于95%。所述方法还用于同时测定处理系统废水中的扑热息痛和双氯芬酸。
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Simultaneous determination of paracetamol and diclofenac in wastewater by high-performance liquid chromatography method
In this study, a simple, selective, and accurate analysis method was developed for the simultaneous determination of anti-inflammatory drugs (paracetamol and diclofenac) existing inlet and outlet of the wastewater treatment system. This method used solid-phase extraction (SPE) and reversed-phase high-performance liquid chromatography with a photodiode array detector (HPLC-PDA). Separation was performed using an HSR C18 column (250 mm × 4.6 mm; 5 µm) with a mobile phase consisting of acetonitrile: sodium dihydrogen orthophosphate in the ratio 60:40 v/v. The flow rate was 1 ml/min, and PDA was detected at 243 nm with paracetamol and 276 nm with diclofenac. The duration of paracetamol and diclofenac was 2.39 and 4.39 min, respectively. The developed method was validated in terms of accuracy, precision, and linearity for two drugs found in the range of 0.01 - 1 µg/ml, and 0.02 - 1 µg/ml for paracetamol, and diclofenac, respectively. The limits of detection for paracetamol and diclofenac were 0.003 µg/ml and 0.006 µg/ml, respectively, whereas the limits of quantification were 0.01 µg /ml and 0.02 µg/ml, respectively. The recoveries for paracetamol and diclofenac were greater than 95 %. The described method also has been applied to determine paracetamol and diclofenac simultaneously in the wastewater of the treatment system.
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