超高效液相色谱-同位素稀释质谱法测定食品中的泛酸

Determination of pantothenic acid in food by ultra performance liquid chromatography-tandem mass spectrometry with isotope dilution

中文关键词:  泛酸  超高效液相色谱-串联质谱法  同位素稀释

英文关键词:pantothenic acid  ultra performance liquid chromatography-tandem mass spectrometry  isotope dilution

中文摘要:

      目的 建立超高效液相色谱-同位素稀释质谱法测定食品中泛酸(pantothenic acid, PA)含量的分析方法。方法 样品中的泛酸用水提取, 经乙酸锌溶液和亚铁氰化钾溶液除杂后, 以乙腈和0.1%甲酸溶液为流动相, 通过Waters HSS T3 C18柱(2.1 mm×100 mm, 1.7 μm)梯度洗脱分离, 流速0.3 mL/min, 进样量2 μL, 柱温35 ℃, 串联质谱检测, 同位素内标法定量。结果 泛酸在10~600 μg/L浓度范围内具有良好的线性关系, 相关系数为0.9999, 方法检出限为0.025 mg/100 g, 定量限为0.075 mg/100 g, 精密度为1.1%~2.1%, 3个加标水平的回收率为98.0%~102.0%, 相对标准偏差为1.7%~3.8%。该方法与微生物法相比结果无明显差异, 且测定时间短, 与高效液相色谱法相比抗干扰能力强。结论 该法操作简单、快速准确, 适用于多种食品中泛酸的测定。

英文摘要:

      Objective To establish a method for determination of pantothenic acid (PA) in food by ultra performance liquid chromatography-tandem mass spectrometry with isotope dilution. Methods PA in sample was extracted by water, then purified by zinc acetate solution and potassium ferricyanide solution. Separation of PA in sample was performed on Waters HSS T3 C18 column (2.1 mm×100 mm, 1.7 μm) with gradient elution. Acetonitrile and 0.1% formic acid solution were used as mobile phase. The flow rate was 0.3 mL/min, the injection volume was 2 μL, and the column temperature was 35 ℃. The analyte was detected by tandem mass spectrometry and quantified by internal standard technique. Results PA had good linearity in the concentration range of 10?600 μg/L, with correlation coefficient as 0.9999. The limit of detection and the limit of quantification for PA were 0.025 mg/100 g and 0.075 mg/100 g, respectively. The relative standard deviations were 1.1%?2.1%. The recoveries of 3 different spiked concentrations were 98.0%?102.0%, the relative standard deviations were 1.7%?3.8%. This method showed no significant difference in results and had shorter measurement time compared to microbiological method. It also had stronger anti-interference ability compared to ultra performance liquid chromatography. Conclusion This method is simple, rapid and accurate, which is suitable for the determination of PA in a variety of foods.