摘要
本文建立超高效液相色谱-串联三重四级杆质谱(UPLC-MS)方法对蛋白型固体饮料中维生素B_(12)的含量进行测定。以醋酸缓冲液为提取液,在沉淀蛋白的过程中通过果胶酶的水解作用降低提取溶液粘度以便采用Strata C18固相萃取柱净化并富集维生素B_(12),富集的洗脱液定容后在以甲酸及甲酸铵为缓冲体系的流动相中经Agilent ZORBA乂SBAq C18高效色谱柱分离,采用大气压电喷雾离子源(ESO在多重反应监测(MRM)模式下以正离子进行定量检测。数据显示维生素B_(12)在1×10^(-9)g/mL-1×10^(-8)g/mL范围内线性关系良好,相关系数大于0.998,平均加标回收率在90%以上,相对标准偏差(RSD)小于5%,具有较高的准确性和良好的重现性。该液质联用方法在蛋白型固体饮料检测方面表现出简便快速的特点,同时具有良好的精密度和准确度。
This paper developed an ultra-performance liquid chromatography mass spectrometer method for determination of the contents of vitamin B_(12)(Cyanocobalamin)in protein solid drink,selects an acetate buffer solution to extract vitamin B_(12),and with the aid of pectase,the viscosity of the extraction was dramatically decreased because of the degradation of polysaccharide,along with protein precipitation.Solid phase extraction(Strata C18)was used for purification and concentration of vitamin B_(12).A mobile phase consisting of formic acid and ammonium formate buffer was applied on Agilent ZORBAX SB-AqC18 column to achieve an excellent separation.Electrospray ionization(ESI)armed with multiple reaction monitoring mode were utilized to quantify vitamin B_(12) with positive ion.Excellent correlation coefficients of the linear curve of vitamin B_(12) were achieved(R>0.998)within the range of 1×10;g/mL-1×10-8 g/mL,the average spike recovery was more than 90%for vitamin B_(12) and RSD was less than 5%,demonstrated the good ruggedness and accuracy.This method is reliable for determination of vitamin B_(12) in protein solid drink because of its excellent accuracy,precision and simplified process.
作者
顾文
林丙文
周亮
李建珍
GU Wen;LIN Bing-wen;ZHOU Liang;LI Jian-zhen(Herbalife(China)Health Products Co.,Ltd.)
出处
《中国标准化》
2022年第4期246-252,共7页
China Standardization
