固相萃取-高效液相色谱法测定红枣制品中环磷酸腺苷  

Determination of Cyclic Adenosine Monophosphate in Jujube Products by Solid-Phase Extraction-High Performance Liquid Chromatography

作　　者：成璐瑶 董朔 张磊[2] 高文涛 李景明[1] 李建贵[2] 马丽艳[1,3] CHENG Lu-yao;DONG Shuo;ZHANG Lei;GAO Wen-tao;LI Jing-ming;LI Jian-gui;MA Li-yan(College of Food Science and Nutritional Engineering,China Agricultural University,Beijing 100083,China;College of Forestry and Landscape Architecture,Xinjiang Agricultural University,Urumqi 830052,China;Quality Inspection and Testing Center for Agri-Products(Beijing),Ministry of Agriculture and Rural Affairs,Beijing 100083,China)

机构地区：[1]中国农业大学食品科学与营养工程学院,北京100083 [2]新疆农业大学林学与风景园林学院,乌鲁木齐830052 [3]农业农村部农产品质量检验测试中心(北京),北京100083

出　　处：《中国调味品》2025年第3期178-183,共6页China Condiment

基　　金：新疆维吾尔自治区重大科技专项(2021A02002-01)。

摘　　要：采用固相萃取-高效液相色谱法建立了红枣制品中环磷酸腺苷(cyclic adenosine monophosphate,cAMP)含量的分析方法。样品提取后,经Strata-X-AW固相萃取柱净化,采用Waters XSelect C18色谱柱(4.6 mm×250 mm,5μm)分离,以甲醇和0.5%甲酸-水溶液为流动相进行梯度洗脱,流速为0.8 mL/min,进样量为10μL。结果表明,cAMP在0.50~50.0 mg/L质量浓度范围内线性关系良好,相关系数(R2)大于0.999。对红枣酸奶、红枣酒、红枣醋等不同种类加工制品进行方法学验证,结果表明,红枣酸奶和红枣酒添加量为5.00,10.0,20.0 mg/kg,红枣醋添加量为2.00,5.00,10.0 mg/kg时,cAMP的平均回收率为86.2%~112%,相对标准偏差为1.7%~5.0%。方法的检出限为0.12~0.46 mg/kg,定量限为0.39~1.55 mg/kg。该方法简便、准确、重复性好、稳定性高,适用于红枣制品中cAMP含量的检测,同时也为产品质量的监管提供了新思路。A method for analyzing the content of cyclic adenosine monophosphate(cAMP)in jujube products is established using solid-phase extraction-high performance liquid chromatography.After extraction,the sample is purified by Strata-X-AW solid-phase extraction column,separated by Waters XSelect C18 chromatographic column(4.6 mm×250 mm,5μm),and gradient elution is performed with methanol and 0.5%formic acid-aqueous solution as the mobile phases at the flow rate of 0.8 mL/min and the sample volume of 10μL.The result show that cAMP has a good linear relationship in the mass concentration range of 0.50~50.0 mg/L,with the correlation coefficient(R2)greater than 0.999.Methodological validation is conducted on different kinds of processed products such as jujube yoghurt,jujube wine and jujube vinegar.The results show that when the addition amount of jujube yogurt and jujube wine is 5.00,10.0,20.0 mg/kg,and the addition amount of jujube wine is 2.00,5.00,10.0 mg/kg,the average recovery rate of cAMP is 86.2%~112%,the relative standard deviation is 1.7%~5.0%,the limits of detection are 0.12~0.46 mg/kg and the limits of quantification are 0.39~1.55 mg/kg.The method is simple and accurate,with good repeatability and high stability.It is suitable for the determination of cAMP content in jujube products,which has provided a new idea for the supervision of product quality.

关 键 词：环磷酸腺苷 红枣 固相萃取 高效液相色谱 

分 类 号：TS207.3[轻工技术与工程—食品科学]