Determination of pantothenic acid, biotin, cyanocobalamine in formula milk powder using ultra performance liquid chromatography-tandem quadrupole mass spectrometry
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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。
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关键词:
- 泛酸 /
- 生物素 /
- 氰钴胺素 /
- 超高效液相色谱-串联质谱法 /
- 奶粉
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. -
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