State Key Laboratory of Organic Geochemistry, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640, China.
Sci Total Environ. 2010 Jul 15;408(16):3424-32. doi: 10.1016/j.scitotenv.2010.03.049. Epub 2010 May 7.
A simultaneous extraction and analysis method was developed for four classes of antibiotics: sulfonamides (SAs), macrolides (MLs), fluoroquinolones (FQs) and tetracyclines (TCs) in sediment. The antibiotics in the sediment were extracted by using an optimized mixed solution (citric buffer: acetonitrile, 50:50 v/v), and analyzed by rapid resolution liquid chromatography-tandem mass spectrometry (RRLC-MS/MS) equipped with electrospray ionization source in the positive mode. The recoveries for the antibiotics in the spiked sediment were: 66.3-123.5%, 48.2-72.0%, 61.8-160.4% and 60.6-151.9% for the SAs, TCs, FQs and MLs, respectively. The LOD ranged from 0.08 microg/kg to 4.2 microg/kg and LOQ from 0.26 microg/kg (erythromycin-H(2)O) to 14.01 microg/kg (norfloxacin). The developed analytical method was applied in the determination of the antibiotics in sediment samples collected from the Pearl Rivers, China. The antibiotics were found at the levels of microg/kg in the sediments of the three rivers. Ofloxacin was found to have the highest concentration of 1560 microg/kg in sediment. However, no significant seasonal variation could be found for the antibiotics in the sediments between wet season and dry season.
建立了一种同时提取和分析沉积物中 4 类抗生素:磺胺类(SAs)、大环内酯类(MLs)、氟喹诺酮类(FQs)和四环素类(TCs)的方法。采用优化的混合溶液(柠檬酸缓冲液:乙腈,50:50v/v)提取沉积物中的抗生素,并用配备电喷雾源的快速分辨液相色谱-串联质谱法(RRLC-MS/MS)在正模式下进行分析。抗生素在加标沉积物中的回收率为:磺胺类、四环素类、氟喹诺酮类和大环内酯类分别为 66.3-123.5%、48.2-72.0%、61.8-160.4%和 60.6-151.9%。LOD 范围为 0.08μg/kg 至 4.2μg/kg,LOQ 范围为 0.26μg/kg(红霉素-H2O)至 14.01μg/kg(诺氟沙星)。该分析方法应用于珠江沉积物中抗生素的测定。在三条河流的沉积物中,抗生素的含量以μg/kg 计。氧氟沙星在沉积物中的浓度最高,为 1560μg/kg。然而,在雨季和旱季之间,沉积物中抗生素的季节性变化并不明显。