超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法检测呕吐物中生物碱
Detection of alkaloids in vomit by ultra-high performance liquid chromatography-quadrupole/electrostatic field orbital trap high resolution mass spectrometry
赵舰 1贺丽迎 1覃梅 1程莉 1唐晓琴 1甘源 1李莉 1何健 1王正虹1
作者信息
- 1. 重庆市疾病预防控制中心/重庆市预防医学科学院,重庆 400707
- 折叠
摘要
目的 采用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱仪,建立呕吐物中生物碱的检测方法.方法 样品经乙腈提取后,以甲醇-乙酸铵(5 mmol/L)水溶液(含0.1％甲酸)为流动相进行梯度洗脱,采用HSS T3色谱柱(100mmx2.1mm,1.8 µm)对待测组分进行色谱分离;采用可加热电喷雾离子源(HESI),全扫描/数据依赖二级质谱扫描(Full MS/ddMS2)模式对待测物进行定性分析;在全扫描模式下以外标法对待测物进行定量检测.结果 在5.0～200.0 μg/L范围内模拟呕吐物中38种生物碱均呈现良好的线性关系,相关系数均＞0.99,检出限0.1～0.5 mg/kg,加标回收率72.9％～111.0％,相对标准偏差5.6％～16.3％.结论 本方法提供了丰富的化合物特征信息,根据一级质谱和二级质谱碎片离子的精确质荷比,在无相关标准品的情况下可对未知化合物进行结构推断和确证;此方法样品前处理简单,定性分析特异性强,定量测定灵敏度高,可满足突发公共卫生事件快速定性、定量检测要求.
Abstract
Objective Using ultra-high performance liquid chromatography-quadrupole/electrostatic field orbital trap high resolution mass spectrometer,to establish a detection method for alkaloids in vomit.Methods After extraction with acetonitrile,the samples were subjected to gradient elution using a methanol ammonium acetate(5 mmol/L)aqueous solution(containing 0.1％formic acid)as mobile phase,and the components were separated by chromatography using an HSS T3 column(100 mmx2.1 mm,1.8 μm);the heated electric spray ionization source(HESI)was used for qualitative analysis of the analytes in the full scanning/data-dependent secondary mass spectrometry(Full MS/ddMS2)mode;then quantify the test substances using the external standard method in full mass mode(full mass).Results The results showed that all the 38 alkaloids in simulated vomit showed a good linear relationship within the range of 5.0～200.0 μg/L,with correlation coefficients greater than 0.99,the detection limits were 0.1～0.5 mg/kg,the spiked recovery rates were 72.9％～111.0％,and the relative standard deviations were 5.6％～16.3％.Conclusion The results suggested that this method provides a wealth of compound characteristic information,based on the precise mass-charge ratio of fragment ions in primary and secondary mass spectrometry,it can infer and confirm the structure of unknown compounds without relevant standards;inaddition,this method has simple sample preparation,strong specificity in qualitative analysis,and high sensitivety in quantitative determination,which could meet the requirements of rapid qualitative and quantitative detection of public health emergencies.
关键词
超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法/生物碱/呕吐物Key words
ultra-high performance liquid chromatography-quadrupole/electrostatic field orbital trap high resolution mass spectrometry/alkaloids/vomit引用本文复制引用
出版年
2024
NETL
NSTL
万方数据