Department of Analytical Chemistry, University of Seville, C/Virgen de África 7, E-41011 Seville, Spain.
J Chromatogr B Analyt Technol Biomed Life Sci. 2012 May 1;895-896:94-101. doi: 10.1016/j.jchromb.2012.03.023. Epub 2012 Mar 28.
Antidiabetic compounds are among the most prescribed pharmaceuticals. Nevertheless, their presence in the environment has been scarcely evaluated as there is no method for their determination in environmental samples. This paper reports the development of an analytical method for the determination of traditionally used antidiabetics (metformin and glibenclamide) and novel antidiabetics (vildagliptin, sitagliptin and pioglitazone). The method is based on solid-phase extraction and determination by high-performance liquid chromatography quadrupole time-of-flight mass spectrometry. The method was applied to effluent wastewater, river water and tap water. Mean recoveries of glibenclamide, vildagliptin, sitagliptin and pioglitazone in the matrices evaluated were in the range 78-83%; limits of quantification were in the range 0.4-4.3 ng L(-1); and precision values were in the range 2.2-13%. The high hydrophilicity and polarity of metformin complicated its simultaneous extraction. Chromabond Tetracycline cartridges and sample pH 8.5 were applied to the extraction of glibenclamide, vildagliptin, sitagliptin and pioglitazone. Oasis HLB cartridges, neutral sample pH and SDS as ion-pair reagent were used for the extraction of metformin. Validation results of metformin were not as favorable as those of the other antidiabetic drugs but were comparable with others previously reported. The developed method was applied to the first-time determination of the concentrations of the five antidiabetic drugs in wastewater, river water and tap water. Metformin was the antidiabetic drug at the highest concentration in wastewater and surface water (up to 253 ng L(-1) and 104 ng L(-1), respectively). Two of the antidiabetic drugs of recent prescription, sitagliptin and vildagliptin, were found in effluent wastewater at concentrations of 117 ng L(-1) and 12 ng L(-1), respectively, and in river water at concentrations of 35 ng L(-1) and 6 ng L(-1), respectively, whereas the classic antidiabetic drug glibenclamide and the novel drug pioglitazone were not detected.
抗糖尿病化合物是最常被开的药物之一。然而，由于目前还没有环境样品中这些化合物的检测方法，因此它们在环境中的存在情况尚未得到充分评估。本文报道了一种用于测定传统抗糖尿病药物（二甲双胍和格列本脲）和新型抗糖尿病药物（维格列汀、西他列汀和吡格列酮）的分析方法的开发。该方法基于固相萃取和高效液相色谱四极杆飞行时间质谱法进行测定。该方法应用于废水、河水和自来水。在所评估的基质中，格列本脲、维格列汀、西他列汀和吡格列酮的平均回收率在 78-83%之间；定量限在 0.4-4.3ng/L 之间；精密度值在 2.2-13%之间。由于二甲双胍的高亲水性和高极性，使其的同时提取变得复杂。Chromabond Tetracycline 萃取小柱和样品 pH8.5 用于提取格列本脲、维格列汀、西他列汀和吡格列酮。Oasis HLB 萃取小柱、中性样品 pH 和 SDS 作为离子对试剂用于提取二甲双胍。二甲双胍的验证结果不如其他抗糖尿病药物理想，但与其他先前报道的结果相当。所开发的方法首次应用于废水中五种抗糖尿病药物浓度的测定，以及河流水和自来水中的浓度测定。在废水和地表水（分别高达 253ng/L 和 104ng/L）中，二甲双胍是浓度最高的抗糖尿病药物。两种最近开的抗糖尿病药物，西他列汀和维格列汀，分别在废水中的浓度为 117ng/L 和 12ng/L，在河水中的浓度为 35ng/L 和 6ng/L。而经典的抗糖尿病药物格列本脲和新型药物吡格列酮则未被检出。
