Batt Angela L, Aga Diana S
Department of Chemistry, State University of New York at Buffalo, 608 Natural Sciences Complex, Buffalo, New York 14260-3000, USA.
Anal Chem. 2005 May 1;77(9):2940-7. doi: 10.1021/ac048512+.
Solid-phase extraction (SPE) and liquid chromatography in combination with ion trap mass spectrometry (LC/MS/MS) conditions were optimized for the simultaneous analysis of 13 antibiotics belonging to multiple classes and caffeine in 3 different water matrixes. The single-cartridge extraction step was developed using a reversed-phase cartridge, resulting in recoveries for the 14 compounds ranging from 71 to 119% with relative standard deviations of 16% or lower. The analytes were separated in one chromatographic run, and the SPE-LC/MS/MS detection limits ranged from 0.03 to 0.19 microg/L. The SPE procedure was validated in groundwater, surface water, and wastewater. The analysis of samples from each of the three water matrixes revealed clindamycin (1.1 microg/L) in surface water and multiple antibiotics in wastewater (0.10-1.3 microg/L). The use of identification points to unambiguously assign the identity of antibiotics in various water matrixes was applied to an ion trap data-dependent scanning method, which simultaneously collects full scan and full scan MS/MS data for the unequivocal identification of target analytes.
对固相萃取(SPE)和液相色谱结合离子阱质谱(LC/MS/MS)条件进行了优化,以同时分析3种不同水基质中属于多个类别的13种抗生素和咖啡因。采用反相柱进行单柱萃取步骤,14种化合物的回收率在71%至119%之间,相对标准偏差为16%或更低。在一次色谱运行中分离分析物,SPE-LC/MS/MS的检测限为0.03至0.19μg/L。该SPE方法在地下水、地表水和废水中得到验证。对三种水基质中的样品进行分析,结果显示地表水中有克林霉素(1.1μg/L),废水中有多种抗生素(0.10 - 1.3μg/L)。将使用识别点明确确定各种水基质中抗生素身份的方法应用于离子阱数据依赖扫描方法,该方法同时收集全扫描和全扫描MS/MS数据,以明确鉴定目标分析物。