Analysis of trace levels of sulfonamide and tetracycline antimicrobials, in groundwater and surface water using solid-phase extraction and liquid chromatography/mass spectrometry
Analysis of trace levels of sulfonamide and tetracycline antimicrobials, in groundwater and surface water using solid-phase extraction and liquid chromatography/mass spectrometry
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DOI：
10.1021/ac010514w
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发表时间：
2001-10-01
影响因子：
7.4
通讯作者：
Thurman, EM
中科院分区：
文献类型：
--
作者：
Lindsey, ME;Meyer, M;Thurman, EM
已经开发了一种方法，用于痕量分析两类抗菌剂，包括六种磺胺类药物（SA）和五种四环素类药物（TC），这些药物通常用于兽医用途和农业饲料添加剂，并被怀疑渗入地下水和地表水。该方法采用固相萃取和液相色谱/质谱（LC/MS）与阳离子电喷雾。金属螯合剂（Na（2）EDTA）与大孔共聚物的独特组合导致在亚微克-升浓度下通过固相萃取的定量回收率（平均回收率，98 +/- 12%）。使用具有甲醇/水梯度的甲酸铵/甲酸缓冲液分离抗菌剂并优化信号强度。确定了每类化合物的质谱裂解和电离特征，以进行明确的鉴定。对于所有SA，鉴别出代表磺胺基片段的特征性m/z 156离子。TC表现出由氨损失引起的17 amu的中性损失和35 amu的中性损失。随后的水分流失。在对美国各地地下水和地表水样品的首次调查中，仅对TC观察到异常的基质效应，要求使用标准加入法对TC进行定量。
A method has been developed for the trace analysis of two classes of antimicrobials consisting of six sulfonamides (SAs) and five tetracyclines (TCs), which commonly are used for veterinary purposes and agricultural feed additives and are suspected to leach into ground and surface water. The method used solid-phase extraction and liquid chromatography/mass spectrometry (LC/MS) with positive ion electrospray. The unique combination of a metal chelation agent (Na(2)EDTA) with a macroporous copolymer resulted in quantitative recoveries by solid-phase extraction (mean recovery, 98 +/- 12%) at submicrogramper-liter concentrations. An ammonium formate/formic acid buffer with a methanol/water gradient was used to separate the antimicrobials and to optimize the signal intensity. Mass spectral fragmentation and ionization characteristics were determined for each class of compounds for unequivocal identification. For all SAs, a characteristic m/z 156 ion representing the sulfanilyl fragment was identified. TCs exhibited neutral losses of 17 amu resulting from the loss of ammonia and 35 amu. from the subsequent loss of water. Unusual matrix effects were seen only for TCs in this first survey of groundwater and surface water samples from sites around the United States, requiring that TCs be quantitated using the method of standard additions..