刘春霞，段国霞，刘丽君，宫慧丽，武伦玮，陈 静，刘 旺，唐 烁，李翠枝*，吕志勇
（内蒙古伊利实业集团股份有限公司，国家市场监管重点实验室（乳及乳制品检测与监控技术），内蒙古 呼和浩特 010110）
摘要：β-羟基-β-甲基丁酸钙（简称HMB-Ca）是一种新资源食品原料，具有增加肌肉合成，减少肌肉分解的功能，在包括老年食品在内的多种食品中可以添加，因此，建立一种粉剂产品如乳粉中HMB 含量的检测方法很有必要。本文尝试了乳粉产品中HMB 含量的HPLC 检测方法，样品经水溶解，亚铁氰化钾、乙酸锌沉淀，水定容后，超声提取。采用紫外检测器检测，外标法定量。在C18 色谱柱分离，波长214nm；柱温：20℃；进样量：10μL；流速：1.0mL/min；流动相：A:磷酸二氢钾溶液—乙腈；B:80%乙腈溶液；每100g 奶粉中β-羟基-β-甲基丁酸钙的添加量为0.5g～3g 时，加标回收率为95.1 %～97.2 %，本方法的方法检出限：0.1g/100g，定量限：0.5g/100g。虽然其检测精度尚待提高，但已基本可以用于HMB 含量较高产品的检测。该方法具有结果准确，处理方法快速简便，重复性好等优点，可用于乳粉中β-羟基-β-甲基丁酸钙的检测。关键词：液相色谱法；乳粉；β-羟基-β-甲基丁酸钙
Determination of the Content of Calcium β-hydroxy-β-methylbutyrate in Milk Powder was Determinedby Liquid Chromatography
LIU Chun-xia，DUAN Guo-xia，LIU Li-jun，GONG Hui-li，WU Lun-wei，CHEN Jin，LIU Wang，TANG Shuo，LI Cui-zhi*，LYU Zhi-yong
（Inner Mongolia Yili Industrial Group Co.，Ltd.，Laboratory of Milk and Dairy Products Detectionand Monitoring Technology for State Market Regulation，Hohhot 010010，China）Abstract: Calcium β- hydroxy- β- methylbutyrate is a new resource food raw material，which has the function ofincreasing muscle synthesis and reducing muscle decomposition，and can be added to a variety of food productsincluding elderly food. Hence，it is necessary to establish a detection method for HMB content in powder productssuch as milk powder. In this paper，the HPLC detection method of HMB content in milk powder products wasreported. The samples were dissolved by water，precipitated by potassium ferrocyanide and zinc acetate，and thenextracted by ultrasonic. Ultraviolet detector was used for detection and external standard method for quantification.Separation was performed on a C18 column with a wavelength of 214nm. Column temperature：20℃；Sample injectionvolume：10μL；Flow rate: 1.0mL/min；Mobile phase: A：potassium dihydrogen phosphate solution - acetonitrile；B：80% acetonitrile solution；When the addition amount of β-hydroxy-β-methylbutyrate in every 100g milk powder was0.5g～3g，the standard recovery rate is 95.1%～97.2%. The detection limit of this method is 0.1g/100g，and thequantitative limit is 0.5g/100g. Although its detection accuracy needs to be improved，it can basically be used for thedetection of products with high HMB content. The method has the advantages of accurate results，rapid and simpletreatment，good repeatability and so on. It can be used for the detection of β- hydroxyl - β- methyl butyrate in milkpowder.
Key words: liquid chromatography；milk powder；β-hydroxyl -β -calcium methyl butyrate
中图分类号：TS252.1 文献标志码：A 文章编号：1007-7871（2024）04-0034-05
2024，Vol.27，No.4