离心超滤-高效液相色谱法测定食品中新食品原料吡咯并喹啉醌二钠盐  

Determination of the New Food Ingredient Pyrroloquinoline Quinone Disodium Salt in Foods by Centrifugal Ultrafiltration Coupled with High Performance Liquid Chromatography

作　　者：潘城 吴媛 孟鹏 黄永辉 肖晶 徐敦明 PAN Cheng;WU Yuan;MENG Peng;HUANG Yonghui;XIAO Jing;XU Dunming(National Quality Supervision and Testing Center for Processed Food(Fuzhou),Fujian Inspection and Research Institute for Product Quality,Fuzhou 350002,China;Technical Center of Xiamen Customs,Xiamen 361026,China;China National Center for Food Safety Risk Assessment,Beijing 100022,China)

机构地区：[1]国家加工食品质量检验检测中心(福州),福建省产品质量检验研究院,福建福州350002 [2]厦门海关技术中心,福建厦门361026 [3]国家食品安全风险评估中心,北京100022

出　　处：《食品科学》2025年第8期322-329,共8页Food Science

基　　金：海关总署科研项目(2023HK127);食品安全国家标准项目(spaq-2023-26);福建省科学技术厅社会发展引导性(重点)项目(2023Y0063)。

摘　　要：基于离心超滤新型前处理技术结合高效液相色谱法,建立食品中新食品原料吡咯并喹啉醌二钠盐的测定方法。样品加入乙二胺四乙酸二钠溶液作为稳定液,经提取液提取定容,超滤管离心净化后在RD-C18色谱柱(4.6 mm×150 mm,5μm)上分离,用四丁基溴化铵-磷酸二氢钾混合溶液/乙腈作为流动相进行梯度洗脱,光电二极管阵列检测器进行检测。结果表明,吡咯并喹啉醌二钠盐在0.0400~10.0 mg/L范围内具有良好线性关系,决定系数为0.9998,液体类样品定量限为1.0 mg/kg,酱油、半固体、固体类样品定量限为4.0 mg/kg。该方法的加标回收率范围为82.1%~103.3%,相对标准偏差为0.7%~2.5%。该方法灵敏度高、操作简单快速、定量准确可靠,适用于多种食品基质中吡咯并喹啉醌二钠盐的定量检测。本研究可有效弥补现有食品中吡咯并喹啉醌二钠盐检测方法的不足,同时可为多种类型食品基质中吡咯并喹啉醌二钠盐的日常监管提供有力的技术支撑。This study established a method for the determination of pyrroloquinoline quinone(PQQ)disodium salt,a newly approved food ingredient in China,in foods using centrifugal ultrafiltration as a novel pretreatment technique combined with high performance liquid chromatography(HPLC).Ethylenediaminetetraacetic acid disodium(EDTA-2Na)solution was used as a stabilizing agent in sample extraction.After purification by centrifugal purification,chromatographic separation was accomplished on a RD-C18 column(4.6 mm×150 mm,5μm)with gradient elution using a mobile phase consisting of tetrabutylammonium bromide-potassium dihydrogen phosphate mixed solution and acetonitrile.Detection was carried out using a photodiode array detector.The calibration curve showed good linearity within the concentration range of 0.0400–10.0 mg/L with a determination coefficient of 0.9998.The limit of quantitation(LOQ)was 1.0 mg/kg for liquid samples and 4.0 mg/kg for soy sauce,semi-solid,and solid samples.The recoveries from spiked samples ranged from 82.1%to 103.3%with a relative standard deviation(RSD)ranging from 0.7%to 2.5%.This method was characterized by high sensitivity,simple operation,rapidity and accurate and reliable quantification,and suitable for the quantitative detection of PQQ disodium salt in various food matrices.This research effectively addresses the shortcomings of existing methods for detecting PQQ disodium salt in foods and provide strong technical support for the routine supervision of PQQ disodium salt in various food matrices.

关 键 词：离心超滤 新食品原料 吡咯并喹啉醌二钠盐 高效液相色谱 

分 类 号：O657.7[理学—分析化学]