特殊医学用途全营养配方食品中β-羟基-β-甲基丁酸钙的含量测定

Determination of calcium β-hydroxy-β-methylbutyrate in whole nutritional formula foods for special medical purposes

中文关键词:  特殊医学用途全营养配方食品  β-羟基-β-甲基丁酸钙  外标法  质量控制

英文关键词:whole nutritional formula foods for special medical purposes  β-hydroxy-β-methylbutyrate  external standard method  quality control

中文摘要:

      目的 通过优化样品前处理和色谱条件, 建立高效液相色谱-紫外检测法测定特殊医学用途全营养配方食品中β-羟基-β-甲基丁酸钙含量的分析方法。方法 样品用0.1 mol/L的盐酸溶液提取, 经离心、上清液过滤后, 以0.05 mol/L磷酸二氢钾溶液(pH 3.0)-乙腈(95:5)为流动相, 采用Caprisil C18-P色谱柱(250 mm×4.6 mm, 5 μm)分离, 紫外检测器检测, 外标法定量。结果 β-羟基-β-甲基丁酸钙在0.0947~ 0.9474 mg/L的质量浓度范围内与峰面积呈现良好的线性关系, 决定系数r2为0.9997, 定量限为0.28 μg/g, 检出限为0.09 μg/g。加标回收率在97.08%~101.22%之间, 相对标准偏差为1.20%。结论 该方法操作简单、重复性好、结果可靠, 可满足特殊医学用途全营养配方食品中β-羟基-β-甲基丁酸钙的含量测定, 为产品的质量控制提供有力的技术支撑, 并填补国内特殊医学用途配方食品关于β-羟基-β-甲基丁酸钙质量检测的空白。

英文摘要:

      Objective To establish a method for the determination of calcium β-hydroxy-β-methylbutyrate in whole nutritional food for special medical purposes by high performance liquid chromatography with ultraviolet detection using optimized sample pretreatment and chromatographic conditions. Methods Samples were extracted by 0.1 mol/L HCl solution. After centrifugation and filtration, the separation of β-hydroxy-β-methylbutyrate was performed on a Caprisil C18-P column (250 mm×4.6 mm, 5 μm) with 0.05 mol/L potassium dihydrogen phosphate (pH 3.0)-acetonitrile (95:5) as the mobile phase and quantitated by external standard method with ultraviolet detector. Results A good linear relationship (r2=0.9997) was observed with concentration ranging from 0.0947 to 0.9474 mg/mL, the limit of quantification was 0.28 μg/g, and the limit of detection was 0.09 μg/g. The recoveries of the spiked samples were from 97.08% to 101.22%, the relative standard deviation was 1.20%. Conclusion The method has the advantages of simple, accurate and precise, which can meet the determination of β-hydroxy-β- methylbutyrate in whole nutritional formula foods for special medical purposes, provide technical support for the quality control of the product, and also fill the blank of quality detection of β-hydroxy-β- methylbutyrate in foods for special medical purposes in China.