Andrija Štampar Teaching Institute of Public Health, Mirogojska, 16, Zagreb, Croatia.
Faculty of Pharmacy and Biochemistry, University of Zagreb, A. Kovačića 1, Zagreb, Croatia.
Environ Sci Pollut Res Int. 2017 Oct;24(29):23389-23400. doi: 10.1007/s11356-017-9894-4. Epub 2017 Aug 26.
Sulfonamides, macrolides, torasemide, fumagillin, and chloramphenicol were simultaneously analyzed in surface water samples by using solid-phase extraction (SPE) and reversed-phase (RP) liquid chromatography-electrospray tandem mass spectrometry (LC-ESI-MS/MS). In the pre-concentration and clean-up process, the pH value of samples and volume of the solvent for extraction of analytes from cartridge were optimized. Extraction recoveries were high with values in the range from 62 to 115%. Limits of quantification (LoQ) were in the range from 0.02 to 0.2 μg L. Repeatability of the method was evaluated at LoQ and expressed as relative standard deviation (RSD). Calculated RSDs were low with values in the range from 2.4 to 14.5%. The method was successfully applied for analysis of surface water real samples. Samples were collected along the rivers in Croatia on four sampling sites in 2012 in Danube catchment areas, 19 sampling sites in Danube and Adriatic catchment areas in 2013, and another 19 places in 2014. Altogether, 20 target compounds were analyzed in 148 water samples and detected in 31 samples in range (0.1-5.3) μg L or in 20.1% of samples. The most frequent and highest concentrations were detected for macrolide antibiotics. This is the first attempt of such monitoring in surface waters in Croatia.
磺胺类药物、大环内酯类、托拉塞米、呋喃西林和氯霉素同时采用固相萃取（SPE）和反相（RP）液相色谱-电喷雾串联质谱（LC-ESI-MS/MS）在地表水样品中进行分析。在预浓缩和净化过程中，优化了样品的 pH 值和从柱上萃取分析物的溶剂体积。萃取回收率高，范围在 62%至 115%之间。定量限（LOQ）在 0.02 至 0.2 μg L 之间。在 LOQ 处评估方法的重复性，并表示为相对标准偏差（RSD）。计算出的 RSD 值较低，范围在 2.4%至 14.5%之间。该方法成功应用于地表水实际样品的分析。2012 年在多瑙河流域的四个采样点、2013 年在多瑙河和亚得里亚海流域的 19 个采样点以及 2014 年的另外 19 个地点采集了样本。总共在 148 个水样中分析了 20 种目标化合物，在 31 个水样中检测到（0.1-5.3）μg L 或在 20.1%的样品中检测到。大环内酯类抗生素的检出频率最高，浓度也最高。这是克罗地亚首次尝试对地表水进行此类监测。
