食品中新型酚丁结构类似物的筛查与定量测定  

Screening and Quantitative Determination of New Oxyphenisatin Analogues in Foods

作　　者：张丽萍 张婉梨 林洁纯 张静 雷毅 ZHANG Li-ping;ZHANG Wan-li;LIN Jie-chun;ZHANG Jing;LEI Yi(Guangdong Institute of Food Inspection,Guangzhou 510435,China)

机构地区：[1]广东省食品检验所,广东广州510435

出　　处：《分析测试学报》2024年第9期1409-1416,共8页Journal of Instrumental Analysis

基　　金：广东省市场监督管理局科技项目(2024CS01);广东省科技厅省直部门协同创新重点项目(2019B020208008)。

摘　　要：在非法添加物风险监测过程中,于声称具有减肥功效的压片糖果中发现一种酚丁结构类似物。根据其高分辨质谱碎片离子裂解规律,采用超高效液相色谱-四极杆轨道阱质谱(UPLC-Q-Orbitrap MS)对该物质进行了结构表征,结合核磁共振氢谱(^(1)H NMR)数据,确定该化合物为泻药成分酚丁的衍生物双己酚丁。该物质与双醋酚丁、双丙酚丁互为同系物。建立了酚丁结构类似物双醋酚丁、双丙酚丁和双己酚丁的超高效液相色谱-三重四极杆质谱(UPLC-QQQ MS)测定方法。3种物质在0.5~50 ng/mL范围内线性关系良好,检出限均为0.025 mg/kg,定量下限均为0.050 mg/kg,在压片糖果和固体饮料基质中3个加标水平下的平均回收率为82.6%~114%,相对标准偏差(RSD,n=6)为1.3%~6.6%。该方法前处理简单、灵敏度高、准确度好,适用于食品中非法添加双醋酚丁、双丙酚丁、双己酚丁的测定。A new oxyphenisatin analogue was discovered from a pressed candy claiming to be a weight loss product during the inspecting and monitoring of illegal adulteration.According to the law of ion fragments in the high-resolution mass spectrum of oxyphenisatin analogues,the unknown com⁃pound was characterized by ultra high performance liquid chromatography equipped with quadrupoleorbitrap mass spectrometry(UPLC-Q-Orbitrap MS).Combined with the ^(1)H NMR spectrum,the un⁃known compound was finally identified as oxyphenisatin dihexylester,a derivative of oxyphenisatin known as a cathartic drug.Oxyphenisatin dihexylester was a homologous compound of oxyphenisatin diacetate and oxyphenisatin dipropinate.Ultra high performance liquid chromatography-triple quad⁃rupole mass spectrometry(UPLC-QQQ MS)was applied to the quantification of oxyphenisatin diace⁃tate,oxyphenisatin dipropionate and oxyphenisatin dihexylester.There were good linear relationships for the three analytes in the range of 0.5-50 ng/mL.The limit of detection and limit of quantification were 0.025 mg/kg and 0.050 mg/kg,respectively.Recoveries at three spiked levels in pressed can⁃dies and solid drinks were ranged from 82.6%-114%,with relative standard deviations(RSDs,n=6)of 1.3%-6.6%.The method has the superiorities in simple pretreatment,high sensitivity and good ac⁃curacy,which can be applied to the detection of illegal additive oxyphenisatin diacetate,oxyphenisatin dipropinate and oxyphenisatin dihexylester in foods.

关 键 词：双己酚丁 非法添加 食品 超高效液相色谱 四极杆轨道阱质谱 三重四极杆质谱 

分 类 号：O657.63[理学—分析化学] TS206.3[理学—化学]