摘要
文章旨在建立高效液相色谱法测定运动营养食品中β-羟基-β-甲基丁酸钙(Calcium-β-hydroxy-β-methylbutyrate,HMB-Ca)含量的方法。取样品于50 mL容量瓶中,加入0.1 mol/L盐酸溶液约40mL,超声处理30 min,用0.1 mol/L盐酸溶液定容至50 mL,用0.45μm滤膜过滤,经Phenomenex Gemini C_(18)色谱柱(250 mm×4.6 mm,5μm)分离,以0.01 mol/L庚烷磺酸钠溶液:甲醇(95:5,V:V)为流动相等度洗脱,流速0.8 mL/min,柱温30℃,进样量10μL,二极管阵列检测器214 nm波长采集数据,外标法定量。HMB-Ca在5-1000 mg/L浓度范围内线性良好,相关系数R^(2)为0.99999。3个浓度水平的平均加标回收率在96.9%-98.1%,相对标准偏差(n=6)为0.87%-1.84%,精密度的相对标准偏差(n=6)为0.32%,方法检出限为0.020 g/100 g,定量限为0.050 g/100 g。该方法操作简便、灵敏度高,具有良好的准确度和精密度,适用于运动营养食品中HMB-Ca含量的测定。
The aim is to establish a method for testing calcium β-hydroxy-β-methylbutyrate(HMB-Ca) in sports nutrition food by high performance liquid chromatography.The samples were taken in 50 mL volumetric flask,40 mL of 0.1 mol/L hydrochloric acid solution was added,ultrasonic treatment was carried out for 30 min,and 0.1 mol/L hydrochloric acid solution was volumetric to 50 mL,filtered with 0.45μm filter membrane,separated by Phenomenex Gemini C_(18) column(250 mmx4.6 mm,5μm),and eluted with 0.01 mol/L sodium hexane sulfonate solution:methanol(95:5,V:V)as flow equality degree,the flow rate was 0.8 mL/min,column temperature was 30℃,sample volume injected was 10μL,diode array detector was used to collect data at 214 nm wavelength.The linearity of HMB-Ca was good in the range of 5-1000 mg/L,and the correlation coefficient squared was 0.9999.The average recoveries of the three concentrations were 96.9%-98.1%,the relative standard deviation(RSD)(n=6)was 0.87%-1.84%,and the precisions relative standard deviation(RSD)(n=6)was 0.32%,the detection limit was 0.020 g/100 g,and the quantitative limit was 0.050 g/100 g.The method is simple,sensitive,accurate and suitable for the determination of HMB-Ca in sports nutrition food.
作者
朱桂芳
喻琼
卢鑫
周璇
杨振栋
韦利宏
孙宇
ZHU Guifang;YU Qiong;LU Xin;ZHOU Xuan;YANG Zhendong;WEI Lihong;SUN Yu(Centre Testing International Group Co.,Ltd.,Shenzhen 518101,China)
出处
《食品科技》
CAS
北大核心
2023年第10期248-253,共6页
Food Science and Technology
基金
科技部重点研发计划项目(2018YFB1403300,2018YFB1403305)。
关键词
β-羟基-β-甲基丁酸钙
高效液相色谱法
运动营养食品
calciumβ-hydroxy-β-methylbutyrate
high-performance liquid chromatography
sports nutritionfood
