液相色谱串接质谱仪测定有机茶叶中的苦参碱与氧化苦参碱  

Determination of Matrine and Oxymatrine in Organic Tea by Liquid Chromatography Coupled With Mass Spectrometer

作　　者：李丽[1] Li Li

机构地区：[1]江苏联合职业技术学院镇江分院镇江高等职业技术学校,江苏镇江212000

出　　处：《化工设计通讯》2022年第1期96-99,共4页Chemical Engineering Design Communications

基　　金：江苏高校‘青蓝工程’资助(苏教师2019[3])。

摘　　要：建立了有机茶叶中苦参碱(Matrine)、氧化苦参碱(Oxymatrine)液相色谱串接质谱仪(LC-MS/MS,Liquid Chromatography Tandem Mass Spectrometry)的检测方法,并运用于市售茶叶中苦参碱、氧化苦参碱含量的筛查。样品用水溶解超声萃取后,加入氨水中和茶叶中的酸性物质;水相中加入氯化钠后,用三氯甲烷提取待测组分。氮吹至干后,残渣用乙醇复溶。经过N-丙基乙二胺固体粉末(PSA)净化后,供LCMS/MS测定。目标化合物在一定范围内(0.312~10.0μg/L)线性关系良好,相关系数大于0.999。苦参碱、氧化苦参碱的检出限(LOD,limit of detection)均为1.0μg/kg;定量限(LOQ,limit of quantification)均为2.0μg/kg。在2.0μg/kg,4.0μg/kg,10.0μg/kg加标水平上,苦参碱的回收率70.5%~78.3%,相对标准偏差4.60%~7.80%;氧化苦参碱的回收率93.0%~105%,相对标准偏差3.21%~5.17%。20份茶叶中检出3份阳性结果。结果表明:该方法简便、快速;其精密度、正确度、检出限等参数均能满足欧盟技术规范的要求,已应用于市售茶叶的筛查。Objective:To establish a detection method for Matrine and Oxymatrine in organic tea by liquid chromatography tandem mass spectrometry(LC-MS/MS,Liquid Chromatography Tandem Mass Spectrometry),and apply it to Screening of matrine and oxymatrine content in teas sold in the market.Method:After dissolving the sample in water and ultrasonically extracting it,adding ammonia water to neutralize the acidic substances in the tea;after adding sodium chloride to the water phase,extract the components to be tested with chloroform.After the nitrogen was blown to dryness,the residue was reconstituted with ethanol.After purification by N-propyl ethylenediamine solid powder(PSA),it is used for LC-MS/MS determination.Results:The target compound has a good linear relationship within a certain range(0.312~10.0μg/L),and the correlation coefficient is greater than 0.999.The limit of detection(LOD,limit of detection)for matrine and oxymatrine are both 1.0μg/kg;the limit of quantification(LOQ,limit of quantification)is both 2.0μg/kg.At the spiked levels of 2.0μg/kg,4.0μg/kg,10.0μg/kg,the recovery rate of matrine is 70.5%~78.3%,and the relative standard deviation is 4.60-7.80%;the recovery rate of oxymatrine is 93.0%~105%,the relative standard deviation is 3.21%~5.17%.Three positive results were detected in 20 teas.Conclusion:The method is simple and fast;its precision,accuracy,detection limit and other parameters can meet the requirements of EU technical specifications,and it has been applied to the screening of commercially available tea.

关 键 词：苦参碱 氧化苦参碱 液相色谱串接质谱 茶叶 

分 类 号：TS272.7[农业科学—茶叶生产加工]