分析测试学报2012，Vol.31Issue(1)：90-95,6.DOI:10.3969/j.issn.1004-4957.2012.01.017
超高效液相色谱-串联质谱联用法同步检测抗生素生产废水中螺旋霉素与新螺旋霉素残留
Simultaneous Determination of Spiramycin and Neospiramycin in Antibiotic Production Wastewater by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
摘要
Abstract
An ultra performance liquid chromatography - tandem mass spectrometric ( UPLC - MS/ MS) method was developed for the simultaneous determination of spiramycin ( e. G. Spiramycin I , SPM- I ) and neospiramycin ( e. G. Neospiramycin I , NSPM- I ) residues in antibiotic production wastewater. The factors influencing the recoveries of antibiotics, including organic extractant type, water sample pH value, extraction time and ratio of water sample to organic extractant, were investigated. The target compounds were separated on an ACQUITY UPLC BEH C18 column (100 mm X 2. 1 mm I. D. , 1. 7 μm) by gradient elution using 0. 1% formic acid(A) and acetonitrile( B) as mobile phases at a flow rate of 0. 2 mL/min. The qualification and quantification of target antibiotics were carried out by MS/MS with positive electrospray ionization under multiple reaction monitoring (MRM) mode. The calibration curves were linear over an antibiotic concentration range of 0. 02 -1.00 mg/L with correlation coefficients ( r2) more than 0.999. The recoveries of antibiotics ranged from 70% to 88% with relative standard deviations(RSD, n =6) less than 10% . The detection lim-its(S/N = 3) for SPM- I and NSPM- I were 0. 03 |xg/L and 0. 06 |xg/L, respectively. The developed method was applied in the determination of antibiotic production wastewater from a pharmaceutical manufacturing factory in Wuxi City, with SPM- I of (115. 6 ± 2. 7 ) mg/L and NSPM- I of (5.3 ±0.4) mg/L.关键词
抗生素生产废水/螺旋霉素/新螺旋霉素/超高效液相色谱-串联质谱法Key words
antibiotic production wastewater/ spiramycin/ neospiramycin/ ultra performance liquid chromatography - tandem mass spectrometry分类
化学化工引用本文复制引用
白辉,贲伟伟,周维芝,强志民..超高效液相色谱-串联质谱联用法同步检测抗生素生产废水中螺旋霉素与新螺旋霉素残留[J].分析测试学报,2012,31(1):90-95,6.基金项目
国家高技术研究发展计划(863)资助项目(2009AA063901) （863）
国家自然科学基金资助项目(50878206, 21107127) （50878206, 21107127）
