超高效液相色谱-四极杆-飞行时间质谱法测定养殖水中丁香酚和异丁香酚  

Determination of eugenol and isoeugenol in aquaculture water by ultra performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry

作　　者：王强[1] 王旭峰[1] 赵东豪[1] 黎智广[1] 张英霞 黄珂[1] WANG Qiang;WANG Xufeng;ZHAO Donghao;LI Zhiguang;ZHANG Yingxia;HUANG Ke(South China Sea Fisheries Research Institute,Chinese Academy of Fishery Sciences,Key Laboratory of Aquatic Product Processing,Ministry of Agriculture and Rural Affairs,Guangzhou 510300,China)

机构地区：[1]中国水产科学研究院南海水产研究所,农业农村部水产品加工重点实验室,广州510300

出　　处：《分析试验室》2022年第9期1083-1088,共6页Chinese Journal of Analysis Laboratory

基　　金：“蓝色粮仓科技创新”重点专项(2019YFD0901701)资助。

摘　　要：建立了超高效液相色谱-四极杆-飞行时间质谱法(UPLC-Q-TOF-MS)测定养殖水中丁香酚和异丁香酚。水体样品经过丹磺酰氯(DNCL)快速衍生化处理后,采用ThermoAccucore C18色谱柱(100 mm×2.1 mm,2.6μm)对衍生物进行分离,以乙腈和0.1%甲酸水溶液为流动相进行梯度洗脱,Q-TOF-MS采用正离子全信息串联质谱扫描模式(MS~E)进行数据采集分析。结果表明,丁香酚和异丁香酚在0.1~20μg/L质量浓度范围内具有良好的线性关系,相关系数(r)大于0.995,水体中的加标回收率分别为83.2%~102%和91.8%~104%,相对标准偏差均小于15%,检出限分别为0.02和0.05μg/L,定量限分别为0.05和0.1μg/L。该方法适用于水产养殖水中丁香酚和异丁香酚的快速测定。An analytical method was established for the determination of eugenol and isoeugenol in aquaculture water by ultra performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF-MS).Water samples were derivatized with dansyl chloride.The derivatization products were separated on a ThermoAccucore C18 column(100 mm×2.1 mm,2.6μm)under gradient elution condition utilizing acetonitrile and 0.1%formic acid as mobile phases.Q-TOF-MS operating in mass data using alternating collision cell energy(MS)mode with positive electrospray ionization was used for the identification of analytes.The results showed that the calibration curves for eugenol and isoeugenol were linear in the range of 0.1-20μg/L with the correlation coefficients(r)higher than 0.995.Their recoveries in aquaculture water were 83.2%-102%and 91.8%-104%,respectively,with relative standard deviations(RSDs)less than 15%.The limits of detection were 0.02 and 0.05μg/L and the limits of quantitation were 0.05 and 0.1μg/L,respectively.The method can be applied to the determination of eugenol and isoeugenol in real water samples.

关 键 词：超高效液相色谱-四极杆-飞行时间质谱 丹磺酰氯 养殖水 丁香酚 异丁香酚 

分 类 号：O657.6[理学—分析化学]