超高效液相色谱-串联质谱法测定谷物中的总烟酸

Determination of niacin in cereals by using ultra performance liquid chromatography- tandem mass spectrometry

建立一种快速、准确的测定谷物中总烟酸含量的超高效液相色谱-串联质谱方法。样品加入烟酸-D4同位素内标校正,经氢氧化钠水解,采用HLB固相萃取柱净化后,以10 mmol/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HSS T3液相色谱柱分离,正离子MRM模式进行定性定量分析。实验结果表明,烟酸在0.1-200 ng/mL浓度范围内线性关系良好,相关系数r〉0.999。线性范围内,平均加标回收率为99.3%-102.6%,相对标准偏差在4.24%-4.74%。仪器的检出限为0.04 ng/mL,定量限为0.1 ng/mL。该方法具有灵敏度高、重现性好、分析时间短等优点,可以为谷物中总烟酸含量的测定提供技术支持。

An ultra performance liquid chromatography- tandem mass spectrometry（ UPLC- MS / MS） method for determination of niacin in cereals has been developed. After spiking nicotinic acid- D4 as an internal standard,samples were extracted by sodium hydroxide and purified with solid phase extraction column. The mobile phase consisted of 10 mmol / L ammonium acetate with 0.1% formic acid and acetonitrile. The niacin was identified by multiple reaction monitoring（ MRM）. The results showed a good linear calibration in the range of 0.1 - 200 ng / m L（ r 0.999）,the mean recoveries and the relative standard deviations were 99.3% - 102.6% and 4.24% - 4.74%,respectively.The limit of detection and quantification of niacin were 0.04 ng / m L and 0.1 ng / m L. This method is sensitive,time saving,and suitable for niacin determination in cereal samples.