食品科学 ›› 2020, Vol. 41 ›› Issue (4): 280-286.doi: 10.7506/spkx1002-6630-20190328-350

• 安全检测 • 上一篇    下一篇

Q-Orbitrap高分辨质谱法测定牛奶中赖丙氨酸及其含量随温度变化的规律

聂雪梅,王菡,许秀丽,张峰,陈达   

  1. (1.天津大学精密仪器与光电子工程学院,天津 300072;2.中国检验检疫科学研究院食品安全研究所,北京 100176;3.陕西科技大学食品与生物工程学院,陕西 西安 710021)
  • 出版日期:2020-02-25 发布日期:2020-03-02
  • 基金资助:
    中国检验检疫科学研究院基本科研业务费项目(2017JK005)

Determination of Lysinoalanine in Milk Products by Q-Orbitrap High Resolution Mass Spectrometry and Variation in Its Content with Temperature

NIE Xuemei, WANG Han, XU Xiuli, ZHANG Feng, CHEN Da   

  1. (1. School of Precision Instrument and Opto-Electronics Engineering, Tianjin University, Tianjin 300072, China; 2. Institute of Food Safety, Chinese Academy of Inspection & Quarantine, Beijing 100176, China;3. School of Food and Biological Engineering, Shaanxi University of Science & Technology, Xi’an 710021, China)
  • Online:2020-02-25 Published:2020-03-02

摘要: 建立一种快速、准确测定牛奶中赖丙氨酸的超高效液相色谱-四极杆/静电场轨道阱高分辨率质谱法分析方法。牛奶样品使用盐酸酸解法进行前处理,并选用Ascentis-C8色谱柱(100 mm×4.6 mm,3 μm)对待测物进行分离,以0.1%甲酸溶液和乙腈作为流动相进行梯度洗脱,在全扫描-数据依赖二级扫描模式进行检测。结果表明:赖丙氨酸的精确质量数偏差小于1.0×10-6,在1~200 μg/L范围内线性关系良好,相关系数均大于0.999;牛奶中赖丙氨酸的检出限为0.01 mg/kg,定量限为0.025 mg/kg。加标量分别为0.025、0.1 mg/kg和0.25 mg/kg,样品的回收率为78.7%~117.1%,相对标准偏差为3.64%。同时采用小型模拟加工设备加热液态奶,研究赖丙氨酸在不同加工条件下含量的变化规律。本方法重复性好、准确、灵敏度高,可用于牛奶中赖丙氨酸的定性、定量筛查。

关键词: 超高效液相色谱, 高分辨率质谱, 赖丙氨酸, 牛奶, 检测

Abstract: A rapid method for the determination of lysinoalanine in milk products by ultra-high performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry (UPLC-Q-Exactive Orbitrap HRMS) was developed. Samples were hydrolyzed with hydrochloric acid to remove impurities such as proteins and then separated on an Ascentis C8 column (100 mm × 4.6 mm, 3 μm) by gradient elution using a binary solvent system composed of acetonitrile and 0.1% formic acid in water. The analytes were detected by quadrupole-orbitrap high resolution mass spectrometry in full-MS and data dependent scan (ddMS2) mode. The results showed that the deviation between the theoretical and measured accurate mass to charge ratio of lysinoalanine was lower than 1.0 × 10-6, and a good linear relationship was observed in the concentration range of 1–200 μg/L with a correlation coefficient higher than 0.999. The limit of detection (LOD) was 0.01 mg/kg and the limit of quantitation (LOQ) was 0.025 mg/kg. Recoveries of the method were in the range of 78.7%–117.1% at spiked concentration levels of 0.025, 0.1, and 0.25 mg/kg, and the relative standard deviation (RSD) for precision was 3.64%. The method had high accurate, repeatability and sensitivity, and consequently was suitable for the qualitative and quantitative screening of lysinoalanine in milk products. Furthermore, the pattern of variation in lysinoalanine content of liquid milk processed using small-scale simulated processing equipment at different temperatures was studied.

Key words: utlra-high performance liquid chromatography, high resolution mass spectrometry, lysinoalanine, milk, determination

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