超高效液相色谱串联质谱法检测奶粉中苯甲酸的含量

Determination of benzoic acid in milk powder by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  苯甲酸  超高效液相色谱串联质谱法  奶粉

英文关键词:benzoic acid  ultra performance liquid chromatography-tandem mass spectrometry  milk powder

中文摘要:

      目的 建立一种超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)检测奶粉中苯甲酸(benzoic acid)含量的分析方法。方法 样品经水提取后, 选用Waters Acquity UPLC BEH C18色谱柱(2.1 mm×50 mm, 1.7 μm), 以甲醇和0.1%氨水作为流动相进行梯度洗脱, 电喷雾离子化(electrospray ionizatio, ESI-)及多反应监测模式(multi-reaction monitoring, MRM)进行测定, 外标法定量。结果 苯甲酸在0.04~2.00 μg/mL浓度范围内, 线性关系良好(r2=0.9996), 样品加标回收率为94.92%~109.31%, 定量限为0.06 μg/g, 结果的相对标准偏差为1.69%~6.90%。结论 该方法前处理简单, 稳定性和可靠性好, 具有良好的定性和定量分析能力, 适用于奶粉中苯甲酸含量的检测。

英文摘要:

      Objective To establish a method for the determination of benzoic acid in milk powder by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods After the sample was extracted by water, it was separated with a Waters Acquity UPLC BEH C18 column (2.1 mm×50 mm, 1.7 μm) by gradient elution using methanol and 0.1% ammonia as mobile phase, performed by electrospray ionization (ESI-) and multi-reaction monitoring (MRM), and quantified by external standard method. Results Benzoic acid had a good linear relationship in the concentration range of 0.04?2.00 mug/mL (r2=0.9996). The recoveries of the spiked samples were 94.92%?109.31%, the limit of quantification was 0.06 μg/g, and the relative standard deviations of the results were 1.69%?6.90%. Conclusion This method has simple pretreatment, good stability and reliability, good qualitative and quantitative analysis ability, and is suitable for detecting benzoic acid content in milk powder.