水中52种抗生素全自动固相萃取-超高效液相色谱-串联质谱法测定
Determination of 52 antibiotics in water through a fully automated solid-phase extraction-ultra-high performance liquid chromatography-tandem mass spectrometry system
郝春慧 1崔伟 1骆玲飞 1李琰1
作者信息
- 1. 上海市闵行区疾病预防控制中心理化检验科,上海 201101
- 折叠
摘要
目的 建立饮用水中52种抗生素的全自动固相萃取-超高效液相色谱-串联质谱测定方法.方法 水样加磷酸调节pH值至2,采用固相萃取盘膜对水样中的抗生素进行富集净化,用10mL5％氨化甲醇分两次洗脱,氮气吹至近干,5％甲醇水溶液定容至1 mL,上机分析.选择ACQUITYUPLCBEHC18色谱柱(2.1 × 100mm,1.7 μm)分离,0.1％甲酸水溶液-0.1％甲酸甲醇为流动相进行梯度洗脱,质谱采用正离子扫描多反应监测(MRM)模式.结果 在0.1～100μg/L范围内,所得52种目标分析物的回归方程均具有良好线性关系.方法检出限为0.1～0.6ng/L,加标回收率为65.1％～133.3％,RSD为3.1％～20.5％.结论 该方法操作简单、快速,准确度和精密度均较高,适用于同时检测饮用水中52种抗生素.
Abstract
Objective To develop a fully automated method combining solid-phase extraction with ultra-high performance liquid chromatography tandem mass spectrometry for the determination of 52 types of antibiotics in drinking water.Methods The water samples were adjusted to pH 2 using phosphoric acid.The antibiotics in the water samples were enriched and purified through solid-phase extraction membrane.Subsequently,the samples underwent two elutions with 10 mL of 5％ammonia methanol,followed by nitrogen-assisted drying to near-dryness.Finally,the volume was adjusted to 1 mL using a 5％methanol aqueous solution for analysis purposes.Separation was achieved using an ACQUITY UPLC BEH C18 chromatographic column(2.1x100 mm,1.7 μm).A mobile phase consisting of a gradient elution system comprising of 0.1％formic acid-water-0.1％formic acid methanol was employed for this purpose.Mass spectrometry utilized positive ion scan multiple reaction monitoring(MRM)mode.Results Within the range of 0.1-100 μg/L,all regression equations obtained for the 52 target analytes exhibited satisfactory linear relationships.The method detection limit ranged from 0.1 to 0.6 ng/L,while the recovery rate varied between 65.1％and 133.3％.Additionally,the relative standard deviation(RSD)ranged from 3.1％to 20.5％.Conclusion The established method is a simple,rapid,and highly accurate and precise approach for the simultaneous detection of 52 types of antibiotics in drinking water.
关键词
固相萃取/超高效液相色谱-串联质谱/抗生素Key words
solid-phase extraction/ultra-high performance liquid chromatography-tandem mass spectrometry/antibiotics引用本文复制引用
基金项目
上海市闵行区自然科学基金研究项目(2021MHZ042)
出版年
2024
NETL
NSTL
万方数据