Water Research Analytical Laboratories, PUB, The Toh Tuck Complex, 82, Toh Guan Road East, #C4-13, Singapore 608576, Singapore.
Talanta. 2011 Sep 30;85(4):1751-9. doi: 10.1016/j.talanta.2011.06.068. Epub 2011 Jul 5.
Acidic pharmaceutical residues are pollutants of emerging concern and are generally monitored by HPLC-MS/MS. However, due to the limited separation efficiency of HPLC column and lack of suitable mass transition for confirmation analysis, some interference may not be separated completely and differentiated from ibuprofen, which may cause the results with interference, especially in sample with complex matrix. The objective of this study is to develop a sensitive and reliable method for the determination of acidic pharmaceutical residues in water samples by GC-MS with better resolution by using methylation derivatization and isotope dilution techniques. TMSDM, a mild reagent, was used as the derivatization reagent coupling with the isotope dilution technique, for the first time, to improve the precision and accuracy of the analytical method to determine the pharmaceutical residues in water. The MDLs for the five acidic organic compounds: ibuprofen, gemfibrozil, naproxen, ketoprofen and diclofenac were from 0.7 to 1.1 ng/L, with recoveries ranging from 93 to 110%. Alternative to the HPLC-MS/MS method, the developed GC-MS protocols provides an additional option for the analysis of acidic pharmaceutical residues in water, with better separation efficiency in reducing interferences from complicated sample matrix, for determination of ibuprofen residues.
酸性药物残留是新兴关注的污染物，通常通过 HPLC-MS/MS 进行监测。然而，由于 HPLC 柱的分离效率有限，并且缺乏合适的质量转移用于确认分析，因此一些干扰可能无法完全分离并与布洛芬区分开来，这可能导致存在干扰的结果，特别是在复杂基质的样品中。本研究的目的是开发一种灵敏可靠的方法，通过 GC-MS 结合甲基化衍生化和同位素稀释技术，提高分辨率，以测定水样中的酸性药物残留。TMSDM 是一种温和的试剂，首次用作衍生化试剂，结合同位素稀释技术，提高了分析方法的精密度和准确度，以测定水中的药物残留。五种酸性有机化合物：布洛芬、吉非贝齐、萘普生、酮洛芬和双氯芬酸的 MDL 为 0.7 至 1.1ng/L，回收率在 93%至 110%之间。与 HPLC-MS/MS 方法相比，所开发的 GC-MS 方案为水中酸性药物残留的分析提供了另一种选择，在减少复杂样品基质干扰方面具有更好的分离效率，可用于测定布洛芬残留。
