超高效液相色谱-串联质谱法测定柞蚕中苦参碱和氧化苦参碱残留量的研究  

Determination of Matrine and Oxymatrine Residues in Tussah Silkworm by Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：杨淑芳[1] 辛若竹 丁梅 张春杨 宫田娇 张海东[1] 靳向东 闫吉昌[3] Yang Shufang;Xin Ruozhu;Ding Mei;Zhang Chunyang;Gong Tianjiao;Zhang Haidong;Jin Xiangdong;Yan Jichang(Sericultural Research Institute of Jilin Province,Jilin Jilin 132012,China;Meihekou Center for Food and Drug Control,Meihekou Jilin 135000,China;Department of Chemistry,Northeast Normal University,Changchun 130024,China)

机构地区：[1]吉林省蚕业科学研究院,吉林吉林132012 [2]梅河口市食品药品检验检测中心,吉林梅河口135000 [3]东北师范大学化学学院,长春130024

出　　处：《蚕业科学》2022年第6期522-530,共9页ACTA SERICOLOGICA SINICA

基　　金：吉林省基本科研经费项目(吉财预[2021]0001号);财政部和农业农村部国家现代农业产业技术体系项目。

摘　　要：为建立超高效液相色谱-串联质谱法测定柞蚕中苦参碱、氧化苦参碱残留量分析方法,用80%乙腈水溶液(含0.2%氨水)超声提取样品,经分散固相萃取净化,以Kinetex 2.6μm Biphenyl 100A色谱柱(100 mm×3.0 mm)分离,0.1%甲酸水和0.1%甲酸甲醇为流动相梯度洗脱,电喷雾电离(ESI),正离子模式多反应监测(+MRM)下检测,外标法定量。结果表明,苦参碱、氧化苦参碱在0.1~50.0 ng/mL范围内呈良好的线性关系,相关系数r均大于0.999,加标回收率在64%~118%之间,相对标准偏差均小于11%,苦参碱检出限为0.05μg/kg,氧化苦参碱检出限为0.1μg/kg。该方法具有较高的灵敏度、准确度和重现性,可用于柞蚕中苦参碱、氧化苦参碱残留量的测定,并为相关产品中苦参碱、氧化苦参碱残留量检测提供了方法依据。To establish an ultra-performance liquid chromatography-tandem mass spectrometry method for the determination of matrine and oxymatrine residues in tussah silkworm,the sample was ultrasonically extracted with 80%acetonitrile aqueous solution(containing 0.2%ammonia)and purified by dispersive solid-phase extraction.It was separated on a Kinetex 2.6μm Biphenyl 100Acolumn(100 mm×3.0 mm),gradient eluted with 0.1%formic acid and 0.1%formic acid methanol,detected with electron spray ionization(ESI)and positive ion mode multiple reaction monitoring(+MRM),and quantified by external standard method.The results showed that the matrine and oxymatrine had a good linear relationship in the range of 0.1-50.0 ng/mL.The correlation coefficient r was greater than 0.999,and the recovery rate of standard addition was between 64%and 118%.The relative standard deviation was less than 11%,the detection limit of matrine was 0.05μg/kg,and the detection limit of oxymatrine was 0.1μg/kg.This method has high sensitivity,accuracy,and reproducibility,and can be used for the determination of matrine and oxymatrine residues in tussah silkworm.Also,it provides a method for the determination of matrine and oxymatrine residues in related products.

关 键 词：柞蚕 苦参碱 氧化苦参碱 超高效液相色谱-串联质谱法 

分 类 号：S885.1[农业科学—特种经济动物饲养]