HPLC-MS/MS法检测奶粉中酪蛋白磷酸肽的含量  

Determination of Casein Phosphopeptides in Milk Powder by HPLC-MS/MS

作　　者：杨余语 刘飞 温林凤 刘果[2] 曹庸[2] YANG Yuyu;LIU Fei;WEN Linfeng;LIU Guo;CAO Yong(Greencream Biotech Co.,Ltd.,Guangzhou 510663,China;College of Food Science,South China Agricultural University,Guangdong Provincial Key Laboratory of Nutraceuticals and Functional Foods,Guangdong Natural Active Object Engineering Technology Research Center,Guangzhou 510642,China)

机构地区：[1]广州绿萃生物科技有限公司,广东广州510663 [2]华南农业大学食品学院,广东省功能食品活性物重点实验室,广东省天然活性物工程技术研究中心,广东广州510642

出　　处：《现代食品》2022年第23期189-194,共6页Modern Food

基　　金：国家自然科学基金资助项目(31972078);广东省科技项目(2018B030322010);广东省基础与应用基础研究基金项目(2020A1515010371);广州市农村科技特派员项目(GZKTP201931)。

摘　　要：研究了高效液相色谱-串联三重四极杆质谱(High Performance Liquid Chromatography Tandem Mass Spectrometry,HPLC-MS/MS)对酪蛋白磷酸肽(Casein Phosphopeptides,CPP)的分析检测,建立了HPLC-MS/MS测定奶粉中CPP含量的分析方法。采用调节pH、超声提取、离心和过滤分离等方式进行样品前处理,经过C18色谱柱分离,以0.1%甲酸水溶液、乙腈为流动相,流速为0.6 mL·min^(-1),三重四极杆质谱仪检测,Q1、MS2扫描模式,使用外标法定量。结果表明,CPP在50~125 mg·L^(-1)具有良好的线性关系,相关系数大于0.998,加标回收率为98.7%~103.3%,相对标准偏差满足试验要求。该方法灵敏度高、净化效果好、定量准确,适用于奶粉中CPP含量的检测分析。The determination of casein phosphopeptides(CPP)by high performance liquid chromatography tandem quadrupole mass spectrometry(HPLC-MS/MS)was studied,and a method for the determination of CPP content in milk powder by HPLC-MS/MS was established.The sample was pretreated by pH adjustment,ultrasonic extraction,centrifugation and filtration separation.After separation by C18chromatographic column,0.1%formic acid aqueous solution and acetonitrile were used as mobile phases,the flow rate was 0.6 mL·min^(-1),triple quadrupole mass spectrometer was used for detection,Q1 and MS2 scanning modes were used,and external standard was used for quantitative determination.The results showed that CPP had a good linear relationship between 50 mg·L^(-1)and 125 mg·L^(-1),the correlation coefficient was greater than 0.998,the recovery rate was 98.7%~103.3%,and the relative standard deviation met the test requirements.The method has high sensitivity,good purification effect and accurate quantification,and is suitable for the detection and analysis of CPP content in milk powder.

关 键 词：酪蛋白磷酸肽 高效液相色谱-串联三重四极杆质谱(HPLC-MS/MS) 奶粉 定量 

分 类 号：O657.63[理学—分析化学]