固相萃取-高效液相色谱法测定乳饮料中吡咯喹啉醌二钠盐  

Determination of pyrroloquinoline quinone disodium salt in milk drink by solid phase extraction-high performance liquid chromatography

作　　者：戴琨 公丕学 赵寅 薛霞 丁一 蔡睿琪 徐大玮 崔玉花 王骏 胡梅 刘艳明 DAI Kun;GONG Pixue;ZHAO Yin;XUE Xia;DING Yi;CAI Ruiqi;XU Dawei;CUI Yuhua;WANG Jun;HU Mei;LIU Yanming(Shandong Institute for Food and Drug Control,Key Laboratory of Supervising Technology for Meat and Meat Products for State Market Regulation,Shandong Research Center of Engineering and Technology for Quality Control of Food for Special Medical Purposes,Industrial Technology Foundation Public Service Platform,Jinan 250101,China)

机构地区：[1]山东省食品药品检验研究院,国家市场监管重点实验室(肉及肉制品监管技术),山东省特殊医学用途配方食品质量控制工程技术研究中心,产业技术基础公共服务平台,济南250101

出　　处：《分析试验室》2025年第2期293-298,共6页Chinese Journal of Analysis Laboratory

基　　金：山东省市场监督管理局科研项目(SDSJKJ202310)资助。

摘　　要：建立了固相萃取柱净化-高效液相色谱测定乳饮料中吡咯喹啉醌二钠盐(PQQ-2Na)的方法。样品用乙腈-柠檬酸溶液(pH 5.0)提取,经混合型阴离子固相萃取柱Oasis WAX净化,以甲醇-20 mmol/L甲酸铵溶液为流动相,在Poroshell 120 EC-C18色谱柱上梯度洗脱,高效液相色谱仪荧光检测器(FLD)检测,外标法定量。对样品提取溶剂、净化及浓缩等前处理过程进行了优化,考察了不同色谱柱及流动相的分离效果。结果表明,在FLD检测条件下,PQQ-2Na在0.10~50μg/mL范围内线性关系良好,相关系数为0.9992,检出限为0.3 mg/kg,定量限为1 mg/kg,加标回收率在80.1%~92.2%之间,相对标准偏差(RSD)为1.4%~3.2%。该方法适用于乳饮料中PQQ-2Na的测定。A method for the determination of pyrroloquinoline quinone disodium salt(PQQ-2Na)in milk drink was established by high performance liquid chromatography(HPLC)coupled with solid phase extraction columns.Samples were extracted using an acetonitrile-citric acid solution(pH 5.0)and purified with an Oasis WAX hybrid weak anion solid phase extraction column.The separation was performed on a Poroshell 120 EC-Cis chromatographic column with a gradient elution using methanol and 20 mmol/L ammonium formate solution as the mobile phase.The target compound was detected by HPLC with fluorescence detector(FLD),and quantification was achieved by the external standard method.The extraction solvents and pre-treatment processes,including purification and concentration,were optimized.The separation efficiency of different chromatographic columns and mobile phase conditions were investigated.The results indicated that PQQ-2Na showed a good linear relationship in the range of 0.10-50μg/mL,with the correlation coefficient of 0.9992.The detection limit of PQQ-2Na was 0.3 mg/kg,and the quantification limit was 1 mg/kg.The recoveries were in the range of 80.1%-92.2%,with the relative standard deviations(RSDs)of 1.4%-3.2%.This method is suitable for the detection of PQQ-2Na in milk drink.

关 键 词：高效液相色谱法 吡咯喹啉醌二钠盐 乳饮料 混合型阴离子固相萃取柱 荧光检测器 

分 类 号：O657.7[理学—分析化学]