Department of Chemistry, University of Waterloo, Waterloo, Ontario, N2L 3G1, Canada.
Anal Chim Acta. 2011 Sep 19;702(1):136-43. doi: 10.1016/j.aca.2011.06.040. Epub 2011 Jun 28.
A high efficiency HPLC method was developed by coupling three sub-2 μm columns in series and operating them at high temperature for the separation of selected non-steroidal anti-inflammatory drugs and veterinary antibiotics in environmental samples. The separation was performed at 80°C to reduce the solvent viscosity, thus reducing the column backpressure. The chromatographic performance of high temperature-extended column length HPLC method was used to determine the most widely used non-steroidal anti-inflammatory drugs and veterinary antibiotics such as sulphonamides in wastewater samples. The method could simultaneously determine 24 pharmaceuticals in short analysis time with high efficiency. The method involved pre-concentration and clean-up by solid phase extraction (SPE) using Oasis HLB extraction cartridges. It was validated based on linearity, precision, detection and quantification limits, selectivity and accuracy. Good recoveries were obtained for all analytes ranging from 72.7% to 98.2% with standard deviations not higher than 6%, except for acetaminophen and acetyl salicylic acid, for which low recovery was obtained. The detection limits of the studied pharmaceuticals ranged from 2 to 16 μg L(-1), while limits of quantification were in the range from 7 to 54 μg L(-1) with UV detection.
开发了一种高效 HPLC 方法，通过将三根亚 2μm 柱串联并在高温下操作，可分离环境样品中的选定非甾体抗炎药和兽用抗生素。在 80°C 下进行分离，以降低溶剂粘度，从而降低柱背压。高温扩展柱长 HPLC 方法的色谱性能用于测定废水中最广泛使用的非甾体抗炎药和兽用抗生素，如磺胺类药物。该方法可在短分析时间内高效地同时测定 24 种药物。该方法通过固相萃取 (SPE) 用 Oasis HLB 萃取小柱进行预浓缩和净化。该方法基于线性、精密度、检测限和定量限、选择性和准确性进行了验证。除了对乙酰氨基酚和乙酰水杨酸外，所有分析物的回收率均在 72.7%至 98.2%之间，标准偏差不高于 6%，除了对乙酰氨基酚和乙酰水杨酸，其回收率较低。所研究药物的检测限范围为 2 至 16μg/L，而紫外检测的定量限范围为 7 至 54μg/L。
