苏丹红Ⅱ纯物质中有机杂质的定性和定量分析  

Qualitative and Quantitative Analysis of the Organic Impurities in Sudan Ⅱ

作　　者：邓超[1] 张伟[2] 黄挺[2] 张辉[1] 何雅娟[2] 陶红[2] 全灿[2] 李红梅[2] DENG Chao;ZHANG Wei;HUANG Ting;ZHANG Hui;HE Ya-juan;TAO Hong;QUAN Can;LI Hong-mei(Zhejiang Province Institute of Metrology,Hangzhou 310018,China;Division of Chemical Metrology and Analytical Science,National Institute of Metrology,Beijing 100029,China)

机构地区：[1]浙江省计量科学研究院,浙江杭州310018 [2]中国计量科学研究院化学计量与分析科学研究所,北京100029

出　　处：《质谱学报》2018年第5期615-622,共8页Journal of Chinese Mass Spectrometry Society

基　　金：国家标准物质资源共享服务平台项目(21-APT1702-12);浙江省质量技术监督系统科研项目(20170214)资助

摘　　要：本实验对苏丹红Ⅱ标准物质候选物中的主要有机杂质进行定性、定量分析,采用高效液相色谱-离子阱-飞行时间串联质谱法(HPLC-IT-TOF MS)和液相色谱-三重四极杆串联质谱法(HPLC-MS/MS)对有机杂质进行定性分析,鉴别出杂质1和杂质2分别为苏丹红Ⅰ和溶剂橙2,推导出杂质3和4的可能分子结构为苏丹红Ⅱ的同分异构体。利用液相色谱外标法测定苏丹红Ⅰ和溶剂橙2的含量分别为0.017%、0.258%,相对标准偏差分别为1.6%、2.5%;采用与主成分苏丹红Ⅱ响应因子一致的方法定量分析杂质3和4,其含量分别为0.012%、0.028%,相对标准偏差分别为7.0%、4.9%。本研究可为苏丹红Ⅱ一级标准物质的研制奠定基础,对苏丹红Ⅱ的准确测定具有重要意义。SudanⅡis one of synthetic organic azo-compounds,which is abundantly used in industry for coloring.A variety of foodstuffs contaminated with Sudan dyes have been detected throughout Europe and Asia.This issue has become one focal point for addressing food safety.SudanⅡcould produce aniline and its derivatives,which could attack the hepatocytes and lead to the toxic hepatic disease.For this reason,accurate and reliable determination of SudanⅡin foodstuff is required for the assurance of consumer’s healthiness.But the traceability of SudanⅡhas not been settled yet.Qualitative and quantitative analysis of the major organic impurities in pure SudanⅡwas performed in this work.The related organic impurities were qualitatively determined by high performance liquid chromatography-ion trap-time of flight mass spectrometry(HPLC-IT-TOF MS)and high performance liquid chromatography-triple quadrupole tandem mass spectrometry(HPLC-MS/MS).Full scan of LC/MS in positive ion mode was firstly executed to obtain the m/z values of the molecules.Then LC-MS/MS was carried out on target compounds to obtain as much structural information as possible.According to the first and the second mass spectra,retention time of standard materials and published reports,the impurities in SudanⅡwere identified and their fragmentation pathways were concluded.Four unknown related organic impurities were observed in SudanⅡ.From analysis of possible structures and fragmentation pathways of fragments,impurities 1 and 2 were successfully identified as SudanⅠand Solvent Orange 2,respectively.The results were verified by standards.The possible molecular structures of impurity 3 and 4 were derived as isomers of SudanⅡ.High performance liquid chromatography external standard method was used to determine the contents of the identified organic impurities.The results showed that there are 0.017%SudanⅠwith the RSD of 1.6%and 0.258%Solvent Orange 2 with the RSD of 2.5%in pure SudanⅡsubstance.Impurities 3 and 4 were quantified in accordance wi

关 键 词：苏丹红Ⅱ 有机杂质 高效液相色谱-离子阱-飞行时间/串联质谱法(HPLC-IT-TOF MS) 定性 定量 

分 类 号：O657.63[理学—分析化学]