Simultaneous determination of human and veterinary antibiotics in various environmental matrices by rapid resolution liquid chromatography-electrospray ionization tandem mass spectrometry
Simultaneous determination of human and veterinary antibiotics in various environmental matrices by rapid resolution liquid chromatography-electrospray ionization tandem mass spectrometry
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快速分辨液相色谱-电喷雾电离串联质谱法同时测定各种环境基质中的人用和兽用抗生素
DOI：
10.1016/j.chroma.2012.04.076
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发表时间：
2012-06-29
影响因子：
4.1
通讯作者：
Zhang, Qian-Qian
中科院分区：
文献类型：
--
作者：
Zhou, Li-Jun;Ying, Guang-Guo;Zhang, Qian-Qian
提出了一种稳健和灵敏的分析方法，其中11类抗生素同时提取和测定地表水，泻湖废水，进水，出水，沉积物，粪便和污泥。将不同体积的水样调节至pH 3，加入0.2 g Na（2）EDTA，然后使用Oasis亲油平衡（HLB）柱进行提取。采用乙腈和柠檬酸缓冲液（pH 3）的混合液作为提取液，通过超声和涡旋混合的组合进行固体样品的提取。固体样品的提取物通过使用强阴离子交换柱（SAX）和HLB柱的串联固相萃取（SPE）方法净化，然后使用配备电喷雾电离源的快速分辨液相色谱-串联质谱（RRLC-MS/MS）进行分析。在50种目标化合物中，39、40、36、40、38、33和36种抗生素在地表水、泻湖废水、进水、出水、沉积物、粪便和污泥3种浓度的加标样品中的回收率分别为50-150%。目标化合物的方法定量限（MQLs）除磺胺和胍外，其余5种药物的浓度范围分别为0.52-5.88 ng/L、2.36-65.8 ng/L、1.73-20 ng/L、1.42-9.52 ng/L、0.64-6.67 ng/g（杆菌肽和氯唑西林除外），1.33-17.4纳克/克（盐霉素、甲基盐霉素、莫能菌素、氯唑西林和新生霉素除外）和1.50-28.6 ng/g（盐霉素、甲基盐霉素、莫能菌素和氯唑西林除外）。该方法已成功应用于惠阳污水处理厂的污水和污泥样品中目标化合物的测定，以及南方某猪场的地下水、泻湖污水、粪便和沉积物中目标化合物的测定。(C)2012爱思唯尔有限公司版权所有。
A robust and sensitive analytical method is presented in which 11 classes of antibiotics are simultaneously extracted and determined in surface water, lagoon wastewater, influent, effluent, sediment, manure and sludge. Water samples with different volumes were adjusted to pH 3, added with 0.2 g Na(2)EDTA and then extracted using Oasis hydrophilic-lipophilic balance (HLB) cartridges. Extraction of solid samples was carried out by a combination of ultrasonic and vortex mixing using a mixture of acetonitrile and citric buffer at pH 3 as the extraction solution. The extracts of the solid samples were then cleaned-up by a tandem solid phase extraction (SPE) method using a strong anion exchange cartridge (SAX) and a HLB cartridge, followed by analysis using rapid resolution liquid chromatography-tandem mass spectrometry (RRLC-MS/MS) equipped with electrospray ionization source. Among the 50 target compounds, the recoveries in the range of 50-150% were obtained for 39,40,36, 40, 38, 33 and 36 antibiotics in the spiked samples of surface water, lagoon wastewater, influent, effluent, sediment, manure and sludge with three concentrations, respectively. Method quantification limits (MQLs) for the target compounds (except sulfaguanidine and sulfanilamide) were in the range of 0.52-5.88 ng/L, 2.36-65.8 ng/L, 1.73-20 ng/L, 1.42-9.52 ng/L, 0.64-6.67 ng/g (except bacitracin and cloxacillin), 1.33-17.4 ng/g (except salinomycin, narasin, monensin, cloxacillin and novobiocin) and 1.50-28.6 ng/g (except salinomycin, narasin, monensin and cloxacillin) in surface water, lagoon wastewater, influent, effluent, sediment, manure and sludge, respectively. The developed analytical method was successfully applied in the determination of target compounds in wastewater and sludge samples from Huiyang wastewater treatment plants, and in ground water, lagoon wastewater, manure and sediment collected from a pig farm, in South China. (C) 2012 Elsevier B.V. All rights reserved.