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
高磊 1黄丽坤 1姜冰 2吴岩 2周春卫 3王妍3
作者信息
- 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
- 折叠
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R2均大于0.99.苦参碱方法检出限为0.21 ng·mL-1,定量限为0.69ng·mL-1;氧化苦参碱方法检出限为0.17ng·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.
Abstract
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 R2 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Key words
matrine/oxymatrine/chromatography-tandem mass spectrometry(LC-MS/MS)/carp/matrix effect引用本文复制引用
出版年
2024
NETL
NSTL
万方数据