摘要
建立了海水中9种大环内酯类抗生素同时测定的液相色谱-四极杆/静电场轨道阱高分辨质谱检测方法。采用Empore C18固相萃取膜提取海水中大环内酯类抗生素,Hypersil GOLD C18色谱柱分离,乙腈和0.005 mol·L^(-1)乙酸铵溶液[含0.1%(体积分数)甲酸]为流动相梯度洗脱。正离子模式下全扫描/数据依赖二级扫描(Full MS/dd-MS2)分析,提取一级质谱准分子离子的精确质量数用于定量分析,二级质谱特征子离子精确质量数用于进一步定性确证。结果表明:9种大环内酯类抗生素均在13 min内出峰,其质量浓度在1~500μg·L^(-1)内与其峰面积响应值呈线性关系,方法的检出限(3S/N)为0.02~0.12 ng·L^(-1)。以空白海水为基体,在3个浓度水平下进行加标回收试验,测得回收率为79.0%~105%,测定值的相对标准偏差(n=6)小于7.5%。方法用于测定25个海水样品中9种大环内酯类抗生素的含量,罗红霉素(ROM)、克拉霉素(CLM)、阿奇霉素(AZM)、替米考星(TMC)均被不同程度地检出。
A method was established for the simultaneous determination of 9 macrolide antibiotics in seawater by liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry. Empore C18 solid phase extraction film was used to extract macrolide antibiotics from seawater. The analytes were seperated by Hypersil GOLD C18 chromatographic column and gradient eluted with the mixtures of acetonitrile and 0.005 mol·L^(-1) ammonium acetate solution [containing 0.1%(φ) formic acid], and analyzed in full scan/data dependent MS2(Full MS/dd-MS2) mode. The results showed that the retention times of 9 macrolide antibiotics were all within 13 min. Linearity relationships between values of mass concentration of 9 macrolide antibiotics and their peak area responses were kept in the range of 1-500 μg·L^(-1), with detection limits(3 S/N) in the range of 0.02-0.12 ng·L^(-1). Recovery was tested by standard addition method using a negative seawater sample as matrix at the 3 concentration levels, giving values of recovery in the range from 79.0% to 105% and of RSDs(n=6) of determined values lower than 7.5%. The proposed method was applied to the determination of 9 macrolide antibiotics in 25 samples of seawater, and ROM, CLM, AZM, and TMC were detected in varying degrees.
作者
吴明媛
余焘
谢宗升
庞燕飞
黄国秋
黄鸾玉
杨姝丽
WU Mingyuan;YU Tao;XIE Zongsheng;PANG Yanfei;HUANG Guoqiu;HUANG Luanyu;YANG Shuli(Guangxi Academy of Fishery Sciences,Nanning 530021,China;Soil and Fertilizer Working Station of Guangxi Zhuang Autonomous Region,Nanning 530007,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2021年第5期444-449,共6页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
广西重点研发计划(桂科AB16380252)
广西重点研发计划(桂科AB18221097)。
关键词
液相色谱-四极杆/静电场轨道阱高分辨质谱法
大环内酯类抗生素
海水
liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry macrolide antibiotic
seawater
