同位素内标法—超高效液相色谱/串联质谱法测定六堡茶中苦参碱和氧化苦参碱残留量  

Determination the residues of matrine and oxymatrine in Liupao tea by UPLC-MS/MS with isotope internal standard method

作　　者：石金娥 张洪禹 辛若竹 丁梅 奚广生 SHI Jine;ZHANG Hongyu;XIN Ruozhu;DING Mei;XI Guangsheng(School of Food and Pharmaceutical Engineering,Wuzhou College,Wuzhou,Guangxi 543002,China;Liupao Tea Modern Industry College,Wuzhou College,Wuzhou,Guangxi 543002,China;School of Physical Education and Health,Wuzhou College,Wuzhou,Guangxi 543002,China;Meihekou Center for Food and Drug Control,Meihekou,Jilin 135000,China)

机构地区：[1]梧州学院食品与制药工程学院,广西梧州543002 [2]梧州学院六堡茶现代产业学院,广西梧州543002 [3]梧州学院体育健康学院,广西梧州543002 [4]梅河口市食品药品检验检测中心,吉林梅河口135000

出　　处：《食品与机械》2024年第3期89-94,共6页Food and Machinery

基　　金：广西科技重大专项(编号:桂科AA22068085)。

摘　　要：目的:以广西六堡茶为例,建立超高效液相色谱—质谱/质谱(UPLC-MS/MS)分析方法测定苦参碱和氧化苦参碱残留量。方法:样品经乙腈水溶液(80%乙腈+0.2%氨水)超声提取,流动相为0.1%甲酸—水和0.1%甲酸—甲醇溶液,梯度洗脱,内标法定量。结果:苦参碱和氧化苦参碱在0.1~80.0 ng/mL质量浓度范围内呈线性,相关系数均>0.9996,检出限均为1.0μg/kg,定量限均为3.0μg/kg,满足茶叶中苦参碱和氧化苦参碱残留量的监管判定要求。通过加标验证,回收率均为92.0%~104.7%,相对标准偏差(RSD)均<5.4%。结论:试验方法结合净化管净化(147.7 mg PSA,15.1 mg GCB,887.2 mg硫酸镁),以Kinetex 2.6μm Biphenyl 100色谱柱(100 mm×3.0 mm)分离,解决了苦参碱和氧化苦参碱提取回收率低、前处理复杂的问题,使苦参碱和氧化苦参碱出峰良好,抗干扰性强。Objective:Taking Guangxi Liupao tea as an example,an UPLC-MS/MS analysis method with residual amounts of matrine and Oxymatrine was established.Methods:The prepared samples were subjected to optimized acetonitrile aqueous solution(80%acetonitrile+0.2%ammonia water)ultrasonic extraction,mobile phase:formic acid water and formic acid methanol(both 0.1%),gradient elution,and internal standard method quantification.Results:It was linear in the range of 0.1~80.0 ng/mL,r was greater than 0.9996,the detection limits of matrine and oxymatrine were 1.0μg/kg,and the quantitative limits were 3.0μg/kg,which met the regulatory determination requirements for the residue of matrine and oxidative matrine in tea.Through the spike verification,the recovery rate was in the range of 92.0%~104.7%,and the relative standard deviation(RSD)was less than 5.4%.Conclusion:Method combined with purification tube purification(147.7 mg PSA,15.1 mg GCB,887.2 mg magnesium sulfate),using Kinetex 2.6μm Biphenyl 100 chromatographic column(100 mm×3.0 mm)separation solves the problems of low extraction recovery rate and complex pre-treatment of matrine and oxymatrine,so that the symmetrical peak shape and strong anti-interference ability of matrine and oxymatrine.

关 键 词：六堡茶 苦参碱 氧化苦参碱 UPLC-MS/MS 

分 类 号：O657.63[理学—分析化学] TS272.7[理学—化学]