固相萃取净化-高效液相色谱法测定饮料中β-羟基-β-甲基丁酸钙  

Determination of Calciumβ-Hydroxy-β-Methylbutyrate in Beverages by Solid-Phase Extraction and High-Performance Liquid Chromatography

作　　者：张文华 侯建波 陈安 汪鹏 祝泽龙 严颖鹏 何建敏 徐敦明 ZHANG Wen-Hua;HOU Jian-Bo;CHEN An;WANG Peng;ZHU Ze-Long;YAN Ying-Peng;HE Jian-Min;XU Dun-Ming(Hangzhou Customs Technical Center,Hangzhou 310016;Xiamen Customs Technical Center,Xiamen 361013)

机构地区：[1]杭州海关技术中心,杭州310016 [2]厦门海关技术中心,厦门361013

出　　处：《中国口岸科学技术》2025年第3期47-53,共7页China Port Science and Technology

基　　金：海关总署科研项目(2023HK127)。

摘　　要：本研究建立了固相萃取-高效液相色谱法测定饮料中β-羟基-β-甲基丁酸钙含量的分析方法。样品采用水振荡提取,二氯甲烷萃取,经PXA固相萃取柱净化,以乙腈-0.02 mol/L磷酸二氢钾溶液为流动相,采用C_(18)色谱柱分离,以流速1.0 mL/min进行梯度洗脱,二极管阵列检测器检测,外标法定量。研究结果显示,β-羟基-β-甲基丁酸钙在0.020~2.00 mg/mL的浓度范围内线性良好,相关系数为0.9993。3个浓度水平的平均加标回收率在92.4%~105%之间,相对标准偏差为0.22%~2.44%,方法检出限为0.05 g/100g,定量限为0.10 g/100g。结果表明,该方法净化效果好、分离良好、专属性强、重复性好、测定结果准确可靠,可满足饮料中β-羟基-β-甲基丁酸钙的含量测定。A method for the determination of calciumβ-hydroxy-β-methylbutyrate(CaHMB)in beverages by solid phase extraction(SPE)coupled with high-performance liquid chromatography(HPLC)was established.Samples were extracted using water oscillation,followed by dichloromethane extraction and purification on a PXA solid-phase extraction column.The analytes were separated on a C_(18)column with a mobile phase consisting of acetonitrile and 0.02 mol/L potassium dihydrogen phosphate solution.Gradient elution was performed at a flow rate of 1.0 mL/min,and detection was achieved using a diode array detector.Quantification was based on the external standard method.CaHMB exhibited good linearity over the concentration range of 0.020-2.00 mg/mL(R~2=0.9993).The average recoveries at three concentration levels ranged from 92.4%-105%,with relative standard deviations(RSDs)of 0.22%-2.44%.The limit of detection(LOD)was 0.05 g/100 g,and the limit of quantification(LOQ)was 0.10 g/100 g.The method demonstrated good purification efficiency,separation specificity,repeatability,and accuracy,making it suitable for the determination of CaHMB in beverages.

关 键 词：羟基-β-甲基丁酸钙 饮料 固相萃取 高效液相色谱法 

分 类 号：TS207.3[轻工技术与工程—食品科学]