UPLC-Q-Orbitrap HRMS对保健食品中U系列新型合成阿片类物质的快速筛查及定量分析  

Rapid Screening and Analysis of U Series Novel Synthetic Opiates in Health Foods by UPLC-Q-Orbitrap HRMS

作　　者：郭思言 张文华 张晓燕 郑文 景渝 李晓华 程妮郦 何梦婷 GUO Si-Yan;ZHANG Wen-Hua;ZHANG Xiao-Yan;ZHENG Wen;JING Yu;LI Xiao-Hua;CHENG Ni-Li;HE Meng Ting(Technical Center of Chongqing Customs,Chongqing 400000;Technical Center of Hangzhou Customs,Hangzhou 310016;Animal,Plant and Food Testing Center of Nanjing Customs,Nanjing 210000)

机构地区：[1]重庆海关技术中心,重庆400000 [2]杭州海关技术中心,杭州310016 [3]南京海关动植物与食品检测中心,南京210000

出　　处：《中国口岸科学技术》2023年第9期50-60,共11页China Port Science and Technology

基　　金：海关总署科研项目(2021HK206)。

摘　　要：建立了超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(ultra-high performance liquid chromatographyquadrupole/electrostatic field orbitrap high resolution mass spectrometry,UPLC-Q-Orbitrap HRMS)对保健食品中U系列新型合成阿片类物质的定性确证和定量分析方法。标准品用0.1%甲酸乙腈溶解稀释后,利用全扫描-数据依赖二级质谱扫描,建立化合物的碎片谱图库、同位素分布图以及母离子及子离子质荷比等参数,样品采用0.1%甲酸乙腈提取,经分散固相萃取净化后仪器分析,通过与标准谱库等化合物库信息比对,实现对多种U系列新型合成阿片类物质的定性确证,利用优化的色谱质谱条件对待测物进行准确定量分析。结果表明,在片剂、茶粉、饮料、糖浆4种不同基质的保健食品中检出限分别为30μg/kg、15μg/kg、3μg/L和15μg/L,定量限分别为80μg/kg、40μg/kg、8μg/L和40μg/L,平均回收率在68.2%~95.4%之间,RSD为1.6%~9.8%,表明该方法能够对样品中U系列新型合成阿片类物质进行快速定性与定量分析。An ultra-high performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry( UPLC-Q-Orbitrap HRMS) method was established for the qualitative confirmation and quantitative analysis of U series new synthetic opioids in health foods. Standard compounds were dissolved and diluted in 0.1% formic acid-acetonitrile solution. A comprehensive approach combining full scan and data-dependent MS/MS scans was employed to establish a library of fragmentation spectra, isotopic distributions, and precursor-to-product ion ratios for the compounds of interest. the qualitative confirmation of various U-series new synthetic opioid substances was achieved. The optimized chromatographic and mass spectrometry conditions were used for quasi quantitative analysis of the analyte. The samples were extracted with 0.1% formic acid-acetonitrile, purified by dispersive solid-phase extraction and analyzed by instrument. By comparing the information with compound libraries such as standard spectra, the qualitative confirmation of U-series novel synthetic opiates was achieved. Additionally, accurate quantification of target analytes was accomplished using optimized chromatographic and mass spectrometric conditions. The method exhibited that the limits of detection were 30 μg/kg, 15 μg/kg, 3 μg/L, and 15 μg/L and the limits of quantification were 80 μg/kg, 40 μg/kg, 8 μg/L, and 40 μg/L for health products with matrices including tablets, powdered tea, beverages, and syrups, respectively. The average recovery rates ranged from 68.2% to 95.4%, with relative standard deviations ranging from 1.6% to 9.8%. Overall, this method enables rapid qualitative and quantitative analysis of U-series novel synthetic opiates in samples.

关 键 词：U系列新型合成阿片类物质 保健食品 快速筛查 高分辨质谱 

分 类 号：O657.63[理学—分析化学] TS218[理学—化学]