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

作　　者：赵舰[1] 贺丽迎 覃梅[1] 程莉[1] 唐晓琴[1] 甘源[1] 李莉 何健[1] 王正虹[1] ZHAO Jian;HE Liying;QIN Mei;CHENG Li;TANG Xiaoqin;GAN Yuan;LI Li;HE Jian;WANG Zhenghong(Chongqing Center for Disease Control and Prevention/Chongqing Municipal Academy of Preventive Medicine,Chongqing 400707,China)

机构地区：[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

出　　处：《中国工业医学杂志》2024年第6期559-565,共7页Chinese Journal of Industrial Medicine

基　　金：重庆市卫生健康委员会重点项目(2017ZDXM002);2003年重庆市公共卫生重点专科(学科)建设项目(渝卫办发[2023]81号)。

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(100 mm×2.1 mm, 1.8μm)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/ddMS^(2))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5.0~200.0μg/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。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 mm×2.1 mm,1.8μm);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/ddMS^(2))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 5.0~200.0μg/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 

分 类 号：O629.3[理学—有机化学] R595[理学—化学]