摘要
本研究建立了一种实时直接分析(DART)-四极杆-静电场轨道离子阱高分辨质谱(Q-Orbitrap HRMS)法快速筛查食品中非法添加的8种工业染料。使用20μL乙腈润湿的碳纤维束(1 cm,6000根)擦拭样品表面取样,DART-HRMS直接检测。根据不同目标物确定DART离子源温度,高分辨质谱采用正离子模式,首先在全扫描模式下筛查目标化合物的一级精确质量数,随后通过二级质谱进一步确认,每个目标化合物用母离子和2个子离子进行定性分析。对于碱性橙2、碱性橙21、碱性橙22、碱性黄2、碱性品红、孔雀石绿、罗丹明B和罗丹明6G这8种工业染料,测得母离子和子离子的质量数误差均小于3×10^(-6),最低检测限在0.01~0.5 mg/L之间,重现性误差(RSD)不大于22%。使用该方法在疑似添加工业染料的市售黄鱼样品中检出碱性橙2。实验表明,首选的拭子取样部位是鱼鳃部、腹鳍、腹部和尾鳍。该方法具有前处理简单、分析速度快、定性准确的优势,可为食品中非法添加染料的快速筛查提供方法参考。
Industrial dyes are bright in color,low in price,and easy to obtain.They are easy to be added to food by illegal traders for quick profit.Most of these substances have carcinogenic,teratogenic and other effects,which are harmful for human health.The rapid screening and identification of illegally added dyes in food will help to fight against such crimes.In this study,a method of direct analysis in real time(DART)-quadrupole-electrostatic field orbital ion trap high resolution mass spectrometry(Q-Orbitrap HRMS) was established to rapidly screen eight industrial dyes,including alkaline orange 2,alkaline orange 21,alkaline orange 22,alkaline yellow 2,alkaline fuchsin,malachite green,rhodamine B and rhodamine 6G.Three kinds of swabs,carbon fiber,cotton and epoxy resin were tested for sampling,and carbon fiber was selected for its higher concentration effect and lower background interference.A bunch of carbon fiber bundle(1 cm,6 000 pieces) wetted with 20 μL acetonitrile was used to wipe the sample surface,then the swab was analyzed directly by DART-HRMS.The ion source temperature of DART was optimized according to different targets.The positive ion mode was selected for HRMS.The target compound was firstly selected by the accurate m/z value in full scan mode,and then was confirmed by the two characteristic product ions.The mass errors for the eight industrial dyes were less than 3×10^(-6),and the limits of detection were in the range of 0.01-0.5 mg/L.The repeatability error(RSD) was no more than 22%.The method was applied to detect alkaline orange 2 in yellow croaker samples suspected of adding industrial dyes.The qualification results were compared with the results acquired by a national standard method,and DART-HRMS was proved to have the advantages of simple pretreatment,fast analysis and accurate qualitative result.Additionally,different sampling positions on spiked yellow croaker were investigated.It turned out that gill,abdominal fin and abdomen were three parts where dyes were easily deposited,thus these were most efficient parts for swab sampling from the outside of yellow croaker.This method can provide a reference for the rapid screening of illegally added dyes in food.
作者
林佳曼
纪佼佼
武丽娜
孔然
向平
孙其然
LIN Jia-man;JI Jiao-jiao;WU Li-na;KONG Ran;XIANG Ping;SUN Qi-ran(Shanghai Key Laboratory of Forensic Medicine,Shanghai Forensic Service Platform,Academy of Forensic Science,Key Laboratory of Forensic Expertise of the Ministry of Justice,Shanghai 200063,China;School of Forensic Medicine,Shanxi Medical University,Jinzhong 030600,China)
出处
《质谱学报》
EI
CAS
CSCD
北大核心
2023年第5期696-705,I0005,共11页
Journal of Chinese Mass Spectrometry Society
基金
中央科研院所公益项目(GY2023G-7)
上海市司法鉴定专业技术服务平台资助项目(19DZ 2292700)。