CAJ | 학술논문

以罗丹明B为质谱增敏衍生化试剂,标记羟基化合物,通过超声波辅助-分散液液微萃取( Ultrasonic assisted-dispersive liquid-liquid microextraction, UA-DLLME)和罗丹明B衍生化联合的策略,建立了超高效液相色谱三重四极杆质谱检测人参二醇( Panaxadiol, PD)的分析方法。化妆品和人参药材中PD经UA-DLLME进行萃取富集(150μL氯仿作为萃取剂,500μL乙醇作为分散剂,3 min),以罗丹明B为衍生试剂,在N,N-羰基二咪唑(N,N-Carbonyldiimidazole, CDI)和4-二甲氨基吡啶(4-Dimethylaminopyridine, DMAP)的催化作用下,70℃微波辅助衍生反应30 min得到稳定的衍生产物。PD衍生物的多反应监测( Multiple reaction monitoring, MRM)模式质谱测定3 min内完成,方法检出限4.0 ng/L,定量限15.0 ng/L,线性、精密度和回收率良好,与以往报道的方法相比,本方法具有灵敏度高和基质效应低的特点。
이라단명B위질보증민연생화시제,표기간기화합물,통과초성파보조-분산액액미췌취( Ultrasonic assisted-dispersive liquid-liquid microextraction, UA-DLLME)화라단명B연생화연합적책략,건립료초고효액상색보삼중사겁간질보검측인삼이순( Panaxadiol, PD)적분석방법。화장품화인삼약재중PD경UA-DLLME진행췌취부집(150μL록방작위췌취제,500μL을순작위분산제,3 min),이라단명B위연생시제,재N,N-탄기이미서(N,N-Carbonyldiimidazole, CDI)화4-이갑안기필정(4-Dimethylaminopyridine, DMAP)적최화작용하,70℃미파보조연생반응30 min득도은정적연생산물。PD연생물적다반응감측( Multiple reaction monitoring, MRM)모식질보측정3 min내완성,방법검출한4.0 ng/L,정량한15.0 ng/L,선성、정밀도화회수솔량호,여이왕보도적방법상비,본방법구유령민도고화기질효응저적특점。
Invirtueofthestrategyofultrasonic-assisteddispersiveliquid-liquidmicroextraction(UA-DLLME) combined with Rhodamine B derivatization, a new ultrahigh performance liquid chromatography-triple quadrupole mass spectrometry ( UHPLC-MS/MS) method was devepled for the sensitive determination of Panaxadiol ( PD) . UA-DLLME and derivatization conditions were investigated. PD in cosmetics and ginseng was extracted by UA-DLLME (150 μL of chloroform as extraction solvent and 500 of μL ethanol as disperser solvent, 3 min) . Using Rhodamine B as precolumn derivatization reagent, the stable derivative of PD was obtained in acetonitrile at 70 ℃ for 30 min under microwave radiation (800 W) with the catalyst of N,N'-carbonyldiimidazole ( CDI) and 4-dimethylaminopyridine ( DMAP) . And then the PD derivative was separated and detected within 3 min by multiple reaction monitoring ( MRM ) mode of UHPLC-MS/MS. LOD was 4. 0 ng/L, and the LOQ was 15. 0 ng/L. This method had good linearity, precision and recovery, and showed obvious advantages such as sensitivity and low matrix effect comparing to the previously reported methods.