高效液相色谱-串联质谱法测定环境水样中13种抗生素  

Determination of 13 Antibiotics in Environmental Water Samples by High Performance Liquid Chromatography-Mass Spectrometry

作　　者：邢月 张雯 程刚 程艳 张琳 胡海洋 XING Yue;ZHANG Wen;CHENG Gang;CHENG Yan;ZHANG Lin;HU Haiyang(College of Chemistry and Chemical Engineering,Xinjiang Agricultural University,Urumqi 830052;Xinjiang Environmental Pollution Monitoring and Risk Warning Laboratory,Urumqi 830012;Xinjiang Research Institute of Environmental Protection,Urumqi 830012;College of Life Sciences,Shangrao Normal University,Shangrao 334003;College of Water Conservancy and Civil Engineering,Xinjiang Agricultural University,Urumqi 830052)

机构地区：[1]新疆农业大学化学化工学院,新疆乌鲁木齐830052 [2]新疆环境污染监控与风险预警实验室,新疆乌鲁木齐830012 [3]新疆环境保护科学研究院,新疆乌鲁木齐830012 [4]上饶师范学院生命科学学院,江西上饶334003 [5]新疆农业大学水利与土木工程学院,新疆乌鲁木齐830052

出　　处：《分析科学学报》2023年第2期125-131,共7页Journal of Analytical Science

基　　金：新疆维吾尔自治区重点实验室开放课题(2022D04006);国家自然科学基金(21667030)。

摘　　要：为了高效、灵敏、准确地测定水体中的抗生素,采用固相萃取-高效液相色谱-串联质谱(SPE-HPLC-MS/MS)技术,建立了检测水中4类13种抗生素的分析方法。实验优化了SPE处理条件和HPLC-MS/MS分析方法,水样经过过滤,HLB固相萃取柱富集,用6 mL甲醇和6 mL 5%氨水甲醇进行洗脱净化,以0.1%甲酸-乙腈为流动相梯度洗脱,采用电喷雾电离源,在多反应监测(MRM)、ESI+模式下定性定量分析。研究结果表明:13种目标抗生素在1~200 ng/L线性范围内相关系数R^(2)均大于0.994,检出限和定量限分别为0.12~2.4 ng/L和0.39~7.98 ng/L,回收率为70.32%~108.6%,相对标准偏差(RSD)≤7.2%。应用该方法对西北干旱区典型内陆河的抗生素污染情况进行了研究,有8种抗生素被检出,浓度范围为:0~68.44 ng/L。因此,该方法可用于水体中痕量抗生素的检测。An analytical method was developed for the detection of 13 antibiotics in 4 categories in water by solid phase extraction-high performance liquid chromatography-tandem mass spectrometry(SPE-HPLC-MS/MS),and the SPE processing conditions and HPLC-MS/MS analytical parameters were further optimized.The water samples were filtered,enriched by HLB SPE column,eluted and purified with 6 mL methanol and 6 mL of 5%ammonia methanol,and target antibiotics were separated by HPLC with 0.1%formic acid(A)-acetonitrile(B)as mobile phase for gradient elution,and qualitatively and quantitatively analyzed by MS in multi-reaction monitoring(MRM)and ESI+mode using an electrospray ionization source.The results showed that the correlation coefficients of 13 target antibiotics were good in the linear range of 1-200 ng/L(R^(2)≥0.994).The detection limit and the quantitative limit were 0.12-2.4 ng/L and 0.39-7.98 ng/L respectively.The recovery was 70.32%-108.6%with relative standard deviation≤7.2%.In addition,this method was also used to study the antibiotic pollution in typical inland rivers in northwest arid area of China.Eight antibiotics were detected in the concentration range of ND-68.44 ng/L.Therefore,the method can be used for the determination of trace antibiotics in environmental water samples.

关 键 词：固相萃取 高效液相色谱-串联质谱 抗生素 环境水样 

分 类 号：O657.63[理学—分析化学]