同位素稀释-超高压液相色谱-串联质谱法测定维生素营养液中的泛酸含量

摘要

目的：建立测定维生素营养液中泛酸含量的同位素稀释-超高压液相色谱-串联质谱法(ID-UHPLC- MS/MS)。方法样品经高氯酸水溶液涡旋提取和除杂、超纯水稀释后,以HSS T3色谱柱和0.1%(v：v)甲酸水溶液-乙腈进行梯度洗脱分离,以串联质谱的多反应监测模式检测,内标法定量。结果泛酸在5~1000µg/L范围内具有良好的线性关系,相关系数(R2)为0.9998；方法检出限为0.02 mg/100 g,定量限为0.07 mg/100 g,3个添加水平的回收率为93.4%~105%,相对标准偏差(n=6)为2.3%~4.4%,日间相对标准偏差(n=3)为2.72%。结论本方法操作简便、分析速度快、灵敏度高、重复性好,为维生素营养液中泛酸含量的定性定量分析提供了可靠的依据。%Objective To develop a simple and rapid method for determination of pantothenic acid in multivitamin supplement by ultra high performance liquid chromatography - tandem mass spectrometry with isotope dilution (ID-UHPLC-MS/MS).Methods The sample was extracted and purified by perchloric acid solution, and separated on an HSS T3 UPLC column with acetonitrile and 0.1% formic acid solution as mobile phase under gradient elution mode, then detected with tandem mass spectrometry under ESI at positive and multiple reaction monitoring (MRM) mode. Stable isotope was used as an internal standard for quantification. Results Pantothenic acid has a good linear relationship in the range of 5~1000μg/L, the limit of detection (LOD) and quantitation (LOQ) of the method was 0.02 mg/100 g and 0.07 mg/100 g respectively. The fine recovery (93.4%~105%), the relative standard deviation (2.3%~4.4%,n=6) and inter-day with RSD (2.72%, n=3) of this method were also obtained.Conclusion The proposed method was successfully applied to determine pantothenic acid in multivitamin supplement. Compared with the standard method, the proposed method was sensitive, rapid, and accurate. It provides a rapid approach for the analysis of pantothenic acid in complex matrix multivitamin supplement solution.