减肥食品中酚丁类化合物筛查与质谱裂解规律OA
Screening and fragmentation pattern analysis of oxyphenisatine and its derivatives in dietetic foods
[目的]运用超高效液相色谱(UPLC)和超高效液相色谱—四极杆—飞行时间质谱(UPLC-Q-TOF-MS),建立减肥食品中非法添加酚丁类化合物的筛查方法.[方法]采用标准物质构建紫外光谱库,并通过高分辨质谱建立含保留时间、母离子和特征碎片离子的质谱库.通过二级质谱分析,明确酚丁类化合物的特征裂解途径,确定酚丁类化合物二级质谱特征性碎片离子.并对UPLC-Q-TOF-MS方法的数据分析方法、特异性、检出限和稳健性展开方法学考察.[结果]酚丁类化合物光谱特征相似,特征性碎片离子为m/z 224.070 6和m/z 196.075 7,氯代衍生物特征性碎片离子为m/z 258.032 1和m/z 230.037 2,氟代衍生物为m/z 242.061 1和m/z 214.066 2,检出限为0.5~5.0 mg/kg.实际样品检测中检出一种未知酚丁类化合物,经确认其为一种氟代双醋酚丁.[结论]该方法抗干扰能力强,稳定性好,适用于减肥食品中酚丁类化合物的快速筛查和确证分析.
[Objective]To establish a screening method for illegally added oxyphenisatine and its derivatives in dietetic foods using ultra-performance liquid chromatography(UPLC)and UPLC quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF-MS).[Methods]A UV spectral library was constructed using reference standards,and a high-resolution mass spectral database containing retention time,precursor ions,and characteristic fragment ions was established.Tandem mass spectrometry(MS/MS)was employed to elucidate characteristic fragmentation pathways of oxyphenisatine compounds and to determine their diagnostic fragment ions.The UPLC-Q-TOF-MS method was further evaluated for data processing,specificity,limit of detection(LOD),and robustness.[Results]Oxyphenisatine compounds exhibited similar spectral features,with diagnostic fragment ions at m/z 224.070 6 and m/z 196.075 7.Chlorinated derivatives produced characteristic ions at m/z 258.032 1 and m/z 230.037 2,while fluorinated derivatives yielded ions at m/z 242.061 1 and m/z 214.066 2.The LODs ranged from 0.5 to 5.0 mg/kg.In actual sample analysis,one unknown oxyphenisatine compound was detected and confirmed to be a fluorinated diacetophenbutate.[Conclusion]This method demonstrates strong anti-interference capacity,good stability,and is suitable for the rapid screening and confirmatory analysis of oxyphenisatine compounds in dietetic foods.
李晓芹;王伟;张玲;曹叶中;丁洪流
苏州市食品检验检测中心,江苏 苏州 215000苏州市食品检验检测中心,江苏 苏州 215000苏州市食品检验检测中心,江苏 苏州 215000苏州市食品检验检测中心,江苏 苏州 215000苏州市食品检验检测中心,江苏 苏州 215000
酚丁类化合物减肥食品光谱特征特征碎片裂解规律
oxyphenisatine and its derivativesdietetic foodsspectral characteristicscharacteristic fragment ionsfragmentation patterns
《食品与机械》 2026 (1)
43-49,7
江苏省市场监督管理局科技计划项目(编号:KJ2023057,KJ2025077)苏州市科技计划项目(编号:2022SS30)
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