超高效液相色谱-串联质谱法同时测定配方奶粉中泛酸、生物素和氰钴胺素

李菁菁; 叶润; 崔亚娟; 李全霞; 李东; 路勇; 张卫民; 黄华; 赵茜茜

doi:10.13386/j.issn1002-0306.2015.12.004

超高效液相色谱-串联质谱法同时测定配方奶粉中泛酸、生物素和氰钴胺素

Determination of pantothenic acid, biotin, cyanocobalamine in formula milk powder using ultra performance liquid chromatography-tandem quadrupole mass spectrometry

摘要

摘要: 建立了超高效液相色谱-串联质谱联用技术同时测定配方奶粉中泛酸、生物素和氰钴胺素的方法。样品经水溶超声提取、三氯甲烷除蛋白后,进行超高效液相色谱-串联质谱分析,采用HSS T3液相色谱柱分离,以10mmol/L乙酸铵溶液（含0.1%甲酸）和乙腈作为流动相进行梯度洗脱,采用电喷雾-正离子电离源多反应监测模式进行定性和定量分析。结果表明:泛酸（VB5）的方法定量限为5μg/100g,生物素（VB7）为2μg/100g,氰钴胺素（VB12）为0.2μg/100g;回收率为79.4%⁸7.8%,相对标准偏差为3.3%⁵.3%。泛酸的线性范围0.5¹000ng/m L,生物素为0.2¹0ng/m L,氰钴胺素为0.02¹0ng/m L。该方法分析操作简单、速度快、灵敏度高、重复性好,适用于配方奶粉中泛酸、生物素和氰钴胺素的同时测定。

Abstract: Ultra performance liquid chromatography- tandem quadrupole mass spectrometry ( UPLC- TQMS) method had been developed for the determination for pantothenic acid (VB5) , biotin (VB7) , cyanocobalamine (VB12) in formula milk powder. The samples were ultrasonic extracted by water, and precipitated protein by chloroform for analyzing by UPLC-MSMS. The analytes were separated by HSS T3 column. The mobile phase consisted of 10mmol/L ammonium acetate with 0.1% formic acid and acetonitrile. The samples were identified and quantified by multiple reaction monitoring (MRM) via positive electrospray ionization (ESI+) . The results showed that the limit of quantification of VB5 were 5μg/100 g, VB7were 2μg/100 g, VB12were 0.2μg/100 g. The recoveries at three spiked levels and the relative standard deviations were 79.4%⁸7.8% and 3.3%⁵.3%, respectively. This method was simple, time saving, sensitive and accurate in the determination of VB5, VB7, VB12 in formula milk powder.