高效液相色谱-串联质谱法测定保健食品中 10种水溶性维生素

Determination of 10 kinds of water-soluble vitamins in food supplements by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  高效液相色谱-串联质谱法  保健食品  水溶性维生素

英文关键词:high performance liquid chromatography-tandem mass spectrometry  supplements  water-soluble vitamins

中文摘要:

      目的 建立高效液相色谱-串联质谱法检测保健食品中10种水溶性维生素的分析方法。方法 采用高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS), ACQUITY UPLC HSS T3色谱柱(2.1 mm×100 mm, 1.8 μm), 以0.1%甲酸水溶液为流动相A, 0.1%甲酸的甲醇溶液为流动相B, 梯度洗脱。通过分子离子峰、二级碎片、色谱保留时间等信息, 对保健食品中10种水溶性维生素进行鉴别和定量测定。结果 10种水溶性维生素实现了同时分离与专属鉴定, 维生素B1在0.01~1 μg/mL的浓度范围内线性关系良好(r＞0.995); 维生素C在0.1~50 μg/mL的浓度范围内线性关系良好(r＞0.995); 其他8种维生素在0.01~10 μg/mL的浓度范围内线性关系良好(r＞0.995), 高、中、低不同浓度的加标回收率在80%~120%之间, 精密度在0.3%~3%之间。结论 本方法专属性强、灵敏度高, 结果准确可靠, 可以作为片剂和口服液基质保健食品中检测水溶性维生素的方法参考。

英文摘要:

      Objective To establish a method for the determination of 10 kinds of water-soluble vitamins in food supplements by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The chromatography was performed using an ACQUITY UPLC HSS T3 column (2.1 mm×100 mm, 1.8 μm), with a mobile phase consisting of 0.1% (V:V) formic acid (phase A) and 0.1% (V:V) formic acid methanol solution (phase B) by gradient elution. Ten kinds of water-soluble vitamins (thiamine, riboflavin, calcium pantothenate, vitamin B6, biotin, folic acid, vitamin B12, nicotinic acid, nicotinamide and ascorbic acid) added in supplements were determined qualitatively and quantitatively based on the information of molecular ion mass, specific fragment ions and chromatographic retention. Results Ten kinds of vitamins could be separated and identified simultaneously. There was a good linearity in the range of 0.01~1 μg/mL for thiamine (r>0.995), 0.1~50 μg/mL for ascorbic acid (r>0.995), and 0.01~10 μg/mL for the other 8 kinds of vitamins (r>0.995). The recoveries of high, medium and low concentrations were between 80% and 120%, and the precisions were between 0.3% and 3%. Conclusion This method has been proved to be simple, sensitive and accurate, and can be used as a reference in the detection of water-soluble vitamins in supplements of tablets and oral liquid.