首页|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

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

扫码查看
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>0.999 6,检出限均为1.0 μg/kg,定量限均为3.0 μg/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 Å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.
Determination the residues of matrine and oxymatrine in Liupao tea by UPLC-MS/MS with isotope internal standard method
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 0.999 6,the detection limits of matrine and oxymatrine were 1.0 μg/kg,and the quantitative limits were 3.0 μg/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® 2.6 μm Biphenyl 100 Å chromatographic column(100 mm X 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.

Liupao teamatrineoxymatrineUPLC-MS/MS

石金娥、张洪禹、辛若竹、丁梅、奚广生

展开 >

梧州学院食品与制药工程学院,广西梧州 543002

梧州学院六堡茶现代产业学院,广西梧州 543002

梧州学院体育健康学院,广西梧州 543002

梅河口市食品药品检验检测中心,吉林梅河口 135000

展开 >

六堡茶 苦参碱 氧化苦参碱 UPLC-MS/MS

广西壮族自治区科技重大专项

桂科AA22068085

2024

食品与机械
长沙理工大学

食品与机械

CSTPCD北大核心
影响因子:0.89
ISSN:1003-5788
年,卷(期):2024.40(3)
  • 26