Citation: CHEN Si-Yi, GUO Xin-Yan, ZHU Wei, WANG Na, WANG Ying, KONG De-Yang. Development of Mass Spectrum Fingerprint Extraction Technology for Antibiotics in Surface Water. Chinese Journal of Analytical Chemistry, 2018, 46(2): 178-187. doi: 10.11895/j.issn.0253-3820.170302 [复制]
Development of Mass Spectrum Fingerprint Extraction Technology for Antibiotics in Surface Water
从固相萃取柱、上样样品pH值、洗脱液、定容液四方面优化前处理流程，建立了地表水中喹诺酮类、磺胺类、四环素类、大环内酯类、青霉素类、头孢菌素类以及氨基糖苷类7类共49种抗生素的质谱指纹的提取方法。水样采用MAX-HLB串联柱富集净化，在超高效液相色谱-串联质谱（UPLC-MS/MS）的多反应监测（MRM）模式下进行定性及定量分析。结果表明，各抗生素在0.001~0.5 μg/mL（链霉素为0.01~5 μg/mL）浓度范围内线性关系良好，各目标抗生素的加标回收率为51.7%~94.8%，相对标准偏差为2.2%~9.7%。以3倍和10倍信噪比确定目标抗生素在两种定容液中的检出限以及定量限分别为0.01~3.23 μg/L和0.05~3.43 μg/L以及0.04~10.8 μg/L和0.17~11.4 μg/L。应用此方法对秦淮河和玄武湖的9个位点进行了抗生素污染筛查。
An extract method for the fingerprint feature of 49 kinds of antibiotics belonging to multiple classes in surface water was developed. Water sample was purified and concentrated by tandem dual column (MAX and HLB), and qualitatively and quantitatively analyzed by ultra-high performance liquid chromatography-tandem mass spectrometric (SPE-UPLC-MS/MS) under multiple reaction monitoring (MRM) mode. The pretreatment was optimized in types of SPE column, loading pH, eluent and redissolution for multiclass antibiotics. The results showed that the linearity of target antibiotics was good in the range of 0.001-0.5 μg/mL (0.01-5 μg/mL for streptomycin). The recoveries were from 51.7% to 94.8%, and the relative standard deviations (RSDs) ranged from 2.19% to 9.67%. The limits of detection (LOD, S/N=3) were 0.01-3.23 μg/L and 0.05-3.43 μg/L and the limits of quantification (LOQ, S/N=10) were 0.04-10.8 μg/L and 0.17-11.4 μg/L in different redissolve solutions. This method was applied to the determination of antibiotics in water samples from 9 sites of Qinhuai River and Xuanwu Lake.
HJ/T52-1999, Water Quality-Guidance on Sampling Techniques of Rivers. Standards of State Environmental Protection Administration of China
水质-河流采样指导. 国家环境保护总局标准. HJ/T52-1999