Department of Analytical Chemistry, Faculty of Chemical Engineering and Technology, University of Zagreb, Zagreb, Croatia.
J Sep Sci. 2010 Feb;33(2):258-67. doi: 10.1002/jssc.200900571.
This paper focuses on the investigation of different types of SPE sorbents for the preconcentration of eight veterinary pharmaceuticals from water samples. The pharmaceuticals studied were sulfamethazine, sulfadiazine, sulfaguanidine, trimethoprim, oxytetracycline, enrofloxacin, norfloxacin and penicillin G/procaine. Five different SPE materials (Strata-X, Strata-X-C, Strata SDB-L, Strata C8 and Strata C18) from Phenomenex were compared with Oasis HLB with a view to obtaining the best cartridges for all pharmaceuticals investigated. Extraction efficiency was determined by HPLC with diode array detection (DAD). HPLC-DAD separation and quantification of the selected pharmaceuticals were carried out under gradient elution by a binary mixture of 0.01 M oxalic acid and ACN based on cyano modified column (LiChrosphere 100 CN) from Merck. Strata-X provided the best results in the preconcentration of 100 mL water samples, yielding average pharmaceutical recoveries of higher than 90%, except for sulfaguanidine (76.1%). The developed Strata-X-HLPC-DAD method was validated and applied, for the efficient investigation of reverse osmosis/nanofiltration membranes and for the removal of these eight pharmaceuticals from the production wastewater samples. NF90 and XLE membranes were shown to be the best for the rejection of all investigated pharmaceuticals.
本文重点研究了不同类型的固相萃取（SPE）吸附剂，用于从水样中预浓缩八种兽药。研究的兽药有磺胺嘧啶、磺胺甲恶唑、磺胺胍、甲氧苄啶、土霉素、恩诺沙星、诺氟沙星和青霉素 G/普鲁卡因。本研究比较了 Phenomenex 公司的五种不同 SPE 材料（Strata-X、Strata-X-C、Strata SDB-L、Strata C8 和 Strata C18）与 Oasis HLB，以期获得对所有研究药物都具有最佳效果的萃取柱。萃取效率通过高效液相色谱法（HPLC）与二极管阵列检测（DAD）来确定。采用梯度洗脱，以基于氰基改性柱（Merck 的 LiChrosphere 100 CN）的 0.01 M 草酸和 ACN 的二元混合物，对选定的药物进行 HPLC-DAD 分离和定量。Strata-X 可在预浓缩 100 mL 水样时提供最佳效果，除磺胺胍（76.1%）外，平均药物回收率均高于 90%。所建立的 Strata-X-HLPC-DAD 方法得到了验证和应用，用于有效研究反渗透/纳滤膜，并从生产废水中去除这八种药物。NF90 和 XLE 膜被证明是所有研究药物的最佳截留膜。
