液相色谱-质谱联用法测定保健食品中去甲乌药碱含量  

Determination of Higenamine in Health Foods by Liquid Chromatography Coupled to Tandem Mass Spectrometry

作　　者：殷玮 凌珊 陈迪新 YIN Wei;LING Shan;CHEN Dixin(Guangzhou General Pharmaceutical Research Institite Co.,Ltd.,Guangzhou 510240)

机构地区：[1]广州医药研究总院有限公司,广州510240

出　　处：《食品工业》2024年第12期315-318,共4页The Food Industry

基　　金：国家科技重大专项课题(2018ZX09721-004);广州市海珠区科技计划项目(海科工商2018-01)。

摘　　要：建立一种灵敏可靠的液相色谱-质谱联用法(LC-MS/MS)测定保健食品中去甲乌药碱含量的方法。样品经75%甲醇提取,采用Waters XBridge C18(100 mm×2.1 mm,2.5μm)色谱柱,多反应监测(MRM),ESI正离子电离模式,去甲乌药碱和内标卡马西平的离子对分别为272.1→107.1和237.1→194.1。流动相A为0.1%甲酸水溶液,流动相B为甲醇,梯度洗脱,流速0.3 mL/min。结果显示,去甲乌药碱在0.500~64.0 ng/mL的质量浓度范围内线性关系良好(Y=0.0562+0.0373X,R^(2)=0.9969),对照品和样品的重复性精密度分别为3.54%和4.69%,平均加样回收率为91.66%±1.75%,检出限为0.200 ng/mL,定量限为0.500 ng/mL。试验方法简单快捷(3 min),灵敏度高,可用于不同保健食品中去甲乌药碱浓度的定量检测。Establish a sensitive and reliable analysis method for the determination of higenamine in various health foods by liquid chromatography coupled to tandem mass spectrometry(LC-MS/MS).The samples were extracted with 75%methanol,and analyzed using a Waters XBridge C18(100 mm×2.1 mm,2.5μm)column,multiple reaction monitoring(MRM),and ESI positive ionization mode.The ion pairings of higenamine and internal standard carbamazepine were 272.1→107.1 and 237.1→194.1,respectively.The mobile phase consisted of 0.1%formic acid aqueous solution(A)and methanol(B),with gradient elution at a flow rate of 0.3 mL/min.The results showed that the linear relationship between higenamine was good in the concentration range of 0.500-64.0 ng/mL(Y=0.0562+0.0373X,R^(2)=0.9969),the standardreference and sample precision were 3.54%and 4.69%,the average recovery rate was 91.66%±1.75%,the detection limit was 0.200 ng/mL,and the quantitative limit was 0.500 ng/mL.This rapid(3 min)and sensitive method was suitable for the quantitative analysis of higenamine in various health foods.

关 键 词：去甲乌药碱 液相色谱-质谱联用法(LC-MS/MS) 保健食品 兴奋剂 

分 类 号：R28[医药卫生—中药学]