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.
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)
出处
《分析测试学报》
CAS
CSCD
北大核心
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)。
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
oxyphenisatin dihexylester
illegal addition
food
ultra high performance liquid chro⁃matography
quadrupole-orbitrap mass spectrometry
triple quadrupole mass spectrometry
