首页|UHPLC-MS/MS法测定酱油中的焦谷氨酸

UHPLC-MS/MS法测定酱油中的焦谷氨酸

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建立了测定酱油中焦谷氨酸的超高效液相色谱-串联质谱(UHPLC-MS/MS)分析方法.采用水直接提取样品中的焦谷氨酸,并适当稀释,将供试液用安捷伦InfinityLab Poroshell 120 Aq-C18(φ4.6 mm × 50 mm,2.7 µm)进行色谱分离,使用0.1%甲酸水溶液-0.1%甲酸乙腈溶液流动相体系梯度洗脱.电喷雾离子源正离子(ESI+)模式,多反应监测(MRM)模式进行测定.实验结果显示,焦谷氨酸的线性范围为0.025~2.5 μg/mL,线性关系良好,相关系数(R2)为0.9992,检出限(LOD)和定量限(LOQ)为0.45 mg/kg和1.5 mg/kg.加标样品的回收率在80.7%~101.1%之间,精密度(RSD)(n=6)为2.4%~8.3%.该方法简单高效,灵敏准确,能应用于酱油中焦谷氨酸含量的定量检测.
Determination of Pyroglutamic Acid in Soy Sauce by UHPLC-MS/MS
An analytical method was developed for the determination of pyroglutamic acid in soy sauce by UHPLC-MS/MS.Pyroglutamic acid in the sample was directly extracted by water,appropriately diluted,and subjected to separation on an Agilent InfinityLab Poroshell 120 Aq-C18(φ 4.6 mm x 50 mm,2.7 µm)column.Gradient elution of the analyte was achieved using a mobile phase system comprising 0.1%formic acid aqueous solution and 0.1%formic acid acetonitrile solution,and the detection was carried out under multiple reaction monitoring(MRM)mode via electrospray ionization in positive ion mode(ESI+).The results demonstrated a good linear relationship for pyroglutamic acid across the concentration range of 0.025 to 2.5 μ g/mL,with a correlation coefficients(R2)of 0.9992.Respectively,the limit of detection(LOD)and the limit of quantitation(LOQ)were determined to be 0.45 mg/kg and 1.5 mg/kg.The recovery rates of the spiked samples ranged from 80.7%to 101.1%,with RSDs(n=6)of 2.4%-8.3%.This method is characterized by its simplicity,efficiency,sensitivity,and accuracy,making it suitable for the precise quantitative determination of pyroglutamic acid in soy sauce.

UHPLC-MS/MSPyroglutamic AcidSoy Sauce

黄嘉颖、方丽、李欣洁、林钦恒、舒永红、钟宇强

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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

UHPLC-MS/MS 焦谷氨酸 酱油

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(10)