固相萃取-液相色谱法测定水环境中4种非甾体抗炎药物

Determination of non-steroidal anti-inflammatory drugs in aquatic environment by SPE-HPLC

目的建立专属、灵敏的固相萃取-液相色谱分析方法,测定水环境中4种非甾体抗炎药(酮洛芬、美洛昔康、双氯芬酸、布洛芬)的质量浓度。方法采用固相萃取技术进行样品前处理,用HPLC法测定。色谱柱:C18(200mm×4.6mm,5μm);流动相:乙腈-20mmol.L-1乙酸铵(60∶40),冰乙酸调pH至3.5;流速:1.0mL·min-1;检测波长:263nm。结果各目标分析物在0.5～50.0mg·mL-1范围内线性关系良好,定量下限均为0.5mg·mL-1。精密度(RSD)范围为0.6%～2.0%,萃取回收率大于78.0%,样品溶液在12h内稳定性良好。结论该法简单、灵敏、准确,可用于水环境中多种非甾体抗炎药的分析。

Objective To develop and validate a specific, sensitive and rapid method for the determination of multi-residual non-ster- oidal anti-inflammatory drugs （NSAIDs） （ketoprofen, meloxicam, diclofenac, ibuprofen） in aquatic environment by SPE-HPLC. Method The sample pretreatment was operated by solid phase extraction （SPE）. The determination was performed on a C18 co- lumn（200 mm×4.6 mm, 5μm）, the mobile phase included acetonitrile and 20 mmol· L^-1 ammonium acetate in water, adjusted to pH 3.5 by addition of acetic acid, the flow rate was 1.0 mL ·min^-1 and wavelength was set at 263 nm. Results The linear calibration curves Were obtained over the concentration range of 0.5-50. 0 mg· L^-1. Quantification limit of the method was 0.5mg· L^-1. The range of precision was 0.6%-2.0 %. The method extraction recoveries were higher than 78.0%, and sample solutions were stable within 12 h. Conclusion The method was simple, sensitive, accurate and reliable for determination of NSAIDs in aquatic environment.