摘要
目的 建立高效液相色谱法测定水产品中5种核苷酸的分析方法。方法 通过色谱条件优化和前处理条件选择,样品在4℃条件下,用5%高氯酸溶液均质提取2次,以0.01 mol/L KH2PO_(4)(含1.45 mmol/L四丁基硫酸氢铵, pH=5.0)-乙腈(95:5, V:V)为流动相洗脱,经C18(250 mm×4.6 mm, 5μm)色谱柱分离,紫外检测器检测,标准曲线外标法定量。结果 5种核苷酸在0.1~100.0μg/mL范围内线性关系良好,相关系数大于0.999,检出限和定量限分别为1.0~2.0 mg/kg和3.0~6.0 mg/kg,方法精密度为2.00%~6.87%,加标回收率在92.3%~105.6%之间,批内相对标准偏差为0.63%~7.90%,批间相对标准偏差为1.72%~7.34%。结论 该方法灵敏度高、重复性好,可用于水产品中5种核苷酸的定性定量分析。
Objective To establish a method for the determination of 5 kinds of nucleotides in aquatic products by high performance liquid chromatography.Methods After optimization of chromatographic conditions and selection of pretreatment conditions,the sample was extracted twice with 5%perchloric acid solution at 4℃,and then extracted with 0.01 mol/L KH2PO_(4)(containing 1.45 mmol/L tetrabutyl ammonium bisulfate,pH=5.0)-acetonitrile(95:5,V:V)was eluted by mobile phase,separated by C18(250 mm×4.6 mm×5μm)column,detected by ultraviolet detector,and quantified by external standard method with standard curve.Results The 5 kinds of nucleotides had a good linear relationship in the range of 0.1–100.0μg/mL,and the correlation coefficient was greater than 0.999.The limits of detection and limits of quantitation were 1.0–2.0 mg/kg and 3.0–6.0 mg/kg,respectively,and the precisions were 2.00%–6.87%.The spike recoveries were 92.3%–105.6%,the intra-assay standard deviations were 0.63%–7.90%,and the inter-assay standard deviations were 1.72%–7.34%.Conclusion This method has high sensitivity and good repeatability,and can be used for the qualitative and quantitative analysis of 5 kinds of nucleotides in aquatic products.
作者
张艳红
易倩
张凤枰
杨洁
杨欣怡
ZHANG Yan-Hong;YI Qian;ZHANG Feng-Ping;YANG Jie;YANG Xin-Yi(Sichuan Willtest Technology Co.,Ltd.,Chengdu 610041,China;Facuity of Quality Management and Inspection Quarantine,Yibin University,Yibin 644007,China)
出处
《食品安全质量检测学报》
2026年第1期195-205,共11页
Journal of Food Safety and Quality
基金
国家标准化管理委员会2025年第六批推荐性国家标准计划项目(20251875-T-326)。
关键词
高效液相色谱法
水产品
核苷酸
high performance liquid chromatography
aquatic products
nucleotides
