LC-MS/MS法测定鲤鱼中苦参碱和氧化苦参碱  

LC-MS/MS method for the determination of matrine and oxymatrine in carp

作　　者：高磊 黄丽坤[1] 姜冰 吴岩 周春卫 王妍 GAO Lei;HUANG Likun;JIANG Bing;WU Yan;ZHOU Chunwei;WANG Yan(School of Food Engineering,Harbin University of Commerce,Harbin,150028,China;Harbin Customs Technology Center,Harbin,150028,China;Shimadzu Enterprise Management(China)Co.Ltd.,Shenyang,110000,China)

机构地区：[1]哈尔滨商业大学食品工程学院,哈尔滨150028 [2]哈尔滨海关技术中心,哈尔滨150028 [3]岛津企业管理(中国)有限公司,沈阳110000

出　　处：《环境化学》2024年第6期2149-2152,共4页Environmental Chemistry

摘　　要：建立基于前处理技术结合液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry,LC-MS/MS)对鲤鱼基质中苦参碱和氧化苦参碱残留量测定的分析方法.样品采用乙腈均质提取的萃取方式,用硫酸钠作为除水剂,样品经过C18色谱柱分离,以水-乙腈为流动相,基质匹配标准曲线外标法定量.苦参碱和氧化苦参碱在质量浓度范围1—50 ng·mL^(−1)内,具有良好的线性关系,相关系数R^(2)均大于0.99.苦参碱方法检出限为0.21 ng·mL^(−1),定量限为0.69 ng·mL^(−1);氧化苦参碱方法检出限为0.17 ng·mL^(−1),定量限为0.52 ng·mL^(−1).添加浓度水平1.0、2.0、5.0 ng·mL^(−1),平均回收率为72.5%—108.7%,相对标准偏差(relative standard deviation,RSD,n=6)为4.2%—8.2%.苦参碱和氧化苦参碱的基质效应均表现为抑制.该方法前处理方法简单,灵敏度高,稳定性好,适合鲤鱼基质苦参碱和氧化苦参碱残留量的测定,同时为后续同类样品检测提供参考,也为今后相关标准制定提供数据积累.To establish an analytical method for the determination of matrine and oxymatrine residue in carp substrate based on pre-treatment technology combined with liquid chromatography-tandem mass spectrometry(LC-MS/MS).The samples were separated by C18 chromatographic column with sodium sulfate as dehydrating agent,water acetonitrile as mobile phase,and quantification by matrix matching standard curve external standard method.There was a good linear relationship between matrine and oxymatrine in the concentration range of 1—50 ng·mL^(−1),and the correlation coefficient R^(2) was greater than 0.99.The detection limit of matrine method is 0.21 ng·mL^(−1),and the quantitative limit is 0.69 ng·mL^(−1).The detection limit of oxymatrine method is 0.17 ng·mL^(−1),and the quantitative limit is 0.52 ng·mL^(−1).The average recovery was 72.5%—108.7%and the relative standard deviation(RSD,n=6)was 4.2%—8.2%when the concentration levels were 1.0,2.0 and 5.0 ng·mL^(−1).The matrix effect of matrine and oxymatrine is inhibition.The pretreatment method is simple,sensitive and stable,which is suitable for the determination of matrix matrine and oxymatrine residues in carp.At the same time,it provides reference for the subsequent detection of similar samples and data accumulation for the formulation of related standards in the future.

关 键 词：苦参碱 氧化苦参碱 液相色谱-串联质谱法(LC-MS/MS) 鲤鱼 基质效应 

分 类 号：X-1[环境科学与工程] O6[理学—化学]