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超高效液相色谱-串联质谱法测定枸杞提取物中的甜菜碱

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建立了超高效液相色谱-串联质谱(UHPLC-MS/MS)测定枸杞提取物中甜菜碱的方法.采用50%甲醇超声提取样品中的甜菜碱,用水稀释后,以含 5 mmoL/L 乙酸铵水溶液-乙腈为流动相梯度洗脱,以Agilent InfinityLab Poroshell 120 HILIC(ϕ2.1 mm×150 mm,2.7 μm)为色谱柱分离甜菜碱目标物,并在正离子模式下,采用MRM模式,外标法定量分析.结果显示,在10~500 ng/mL质量浓度范围内,甜菜碱具有良好的线性关系,相关系数(r2)为 0.9994,检出限(LOD)和定量限(LOQ)分别为 0.12 mg/kg 和 0.35 mg/kg.在 3个质量浓度级别的加标水平下,甜菜碱的平均回收率在81.5%~102.7%之间,相对标准偏差(RSD)(n=6)为1.0%~7.5%.方法可行性强、简单快速,具有较高的灵敏度、回收率和精密度,可用于高效检测枸杞提取物中的甜菜碱.
Determination of Betaine in Lycium Barbarum Extract by Ultra Performance Liquid Chromatography-tandem Mass Spectrometry
The experiment aimed to establish a method for the determination of betaine in Lycium barbarum extract by ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS).Betaine in Lycium barbarum extrac sample was extracted ultrasonically with 50%methanol,diluted with water,and separated on an Agilent InfinityLab Poroshell 120 HILIC(ϕ2.1 mm×150 mm,2.7 μm)column with gradient elution using the mobile phases consisting of 5 mmoL/L ammonium acetate aqueous solution and acetonitrile.Quantitative analysis was carried out by electrospray ionizationsource in positive ion mode under multi reaction monitoring(MRM)mode,using external standard method.The results showed good linearity for betaine in the concentration range of 10-500 ng/mL,with a correlation coefficient(r2)of 0.9994.The limits of detection(LOD)and quantitation(LOQ)were 0.12 mg/kg and 0.35 mg/kg,respectively.The spiked experiments were performed at three concentration levels,and the average recovery rates for betaine ranged from81.5%to 102.7%,with relative standard deviations(RSDs)of 1.0%-7.5%(n=6).The study indicates that the method is feasible,simple,rapid,and exhibits high sensitivity,high accuracy,and good reproducibility,making it effective for detecting the concentration of betaine in Lycium barbarum extract.

Ultra Performance Liquid Chromatography-tandem Mass SpectrometryBetaineLycium Barbarum Extract

李洁莹、钟建权、彭静雅、蔡杏宜、林钦恒、潘云山

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广东省绿色产品认证检测中心有限公司,广东 广州 510440

广东省科学院测试分析研究所 (中国广州分析测试中心),广东省化学测量与应急检测技术重点实验室,广东省保健食品功效成分检测与风险物质快速筛查工程技术研究中心,广东 广州 510070

超高效液相色谱-串联质谱法 甜菜碱 枸杞提取物

2024

云南化工
云南省化工研究院 云天化集团有限责任公司 云南煤化工集团有限公司 云南省化学化工学会

云南化工

影响因子:0.272
ISSN:1004-275X
年,卷(期):2024.51(7)