Determination of 51 Hormones in Milk by Ultrahigh Performance Liquid Chromatography-Quadrupole-Time of Flight Mass Spectrometry

DUAN He-jun; ZHANG Jing; SUN Jia-lin; YANG Run-hui; SHAO Bing; NIU Yu-min

doi:10.19969/j.fxcsxb.23062803

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Determination of 51 Hormones in Milk by Ultrahigh Performance Liquid Chromatography-Quadrupole-Time of Flight Mass Spectrometry

Scientific Papers | 更新时间：2023-10-18

- Determination of 51 Hormones in Milk by Ultrahigh Performance Liquid Chromatography-Quadrupole-Time of Flight Mass Spectrometry
- Journal of Instrumental Analysis Vol. 42, Issue 10, Pages: 1319-1326(2023)
- 作者机构：
  
  1.北京市疾病预防控制中心食物中毒诊断溯源技术北京市重点实验室，北京 100013
  2.首都医科大学公共卫生学院，北京 100069
  3.中国农业大学兽医学院，北京 100193
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.23062803
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段鹤君,张晶,孙佳林等.超高效液相色谱-四极杆-飞行时间质谱法测定牛奶中51种激素[J].分析测试学报,2023,42(10):1319-1326.

DUAN He-jun,ZHANG Jing,SUN Jia-lin,et al.Determination of 51 Hormones in Milk by Ultrahigh Performance Liquid Chromatography-Quadrupole-Time of Flight Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(10):1319-1326.
段鹤君,张晶,孙佳林等.超高效液相色谱-四极杆-飞行时间质谱法测定牛奶中51种激素[J].分析测试学报,2023,42(10):1319-1326. DOI： 10.19969/j.fxcsxb.23062803.

DUAN He-jun,ZHANG Jing,SUN Jia-lin,et al.Determination of 51 Hormones in Milk by Ultrahigh Performance Liquid Chromatography-Quadrupole-Time of Flight Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(10):1319-1326. DOI： 10.19969/j.fxcsxb.23062803.

摘要

基于超高效液相色谱-四极杆-飞行时间质谱（UPLC-Q-TOF MS），建立了牛奶中51种激素的高通量筛选和定量方法，并采用信息依赖型采集（IDA）模式建立了51种激素的定性筛选数据库。牛奶样品经乙腈沉淀蛋白后，采用氧化锆包覆硅胶（Z-Sep）填料进一步净化。采用Waters Acquity BEH C,18,（100 mm×2.1 mm，1.7 μm）色谱柱进行分离，UPLC-Q-TOF MS测定，基质匹配曲线外标法定量。牛奶中51种激素的线性范围为0.10~500 μg/L，相关系数（,r,2,）均大于0.99；检出限为0.03~1.67 μg/kg，定量下限为0.10~5.00 μg/kg；在5、10、50 μg/kg加标水平下的回收率为44.6%~120%，相对标准偏差为0.90%~20%。利用该方法测定了20份市售牛奶样品，其中19份样品检出孕酮，检出量为0.80~4.51 µg/kg；1份样品中含有痕量的氢化可的松，检出量为0.62 µg/kg；其他激素均未检出。该方法具有良好的线性、灵敏度、准确度和精密度，可用于多种激素的同时定性定量分析。

Abstract

A comprehensive high-throughput screening and quantification method for hormones was established based on ultrahigh performance liquid chromatography-quadrupole-time of flight mass spectrometry（UPLC-Q-TOF MS）. A database for qualitative screening of 51 hormones was established using information dependent acquisition（IDA） mode. After precipitation of protein in milk samples by acetonitrile，the milk samples were purified using zirconia coated silica gel sorbent（Z-Sep）. Separation was performed on Waters Acquity BEH C,18, column（100 mm × 2.1 mm，1.7 μm） with gradient elution by UPLC-Q-TOF MS and quantified using matrix matching curve external standard method. The method showed good linearity in the range of 0.10-500 μg/L，with correlation coefficients（,r,2,） greater than 0.99. The limits of detection（LODs） and limits of quantitation（LOQs） were in the range of 0.03-1.67 μg/kg and 0.10-5.00 μg/kg，respectively. The recoveries is 44.6%-120% with relative standard deviations of 0.90%-20%. Twenty milk samples were determined using this method，of which 19 samples were detected for progesterone，with content ranged from 0.80 to 4.51 µg/kg，one sample had trace amounts of cortisol detected at 0.62 µg/kg，and no other hormones were detected. This method has good linearity，sensitivity，accuracy，and precision，and can be used for simultaneous qualitative and quantitative analysis of multiple hormones.

关键词

激素牛奶超高效液相色谱-四极杆-飞行时间质谱QuEChERS

Keywords

hormonesmilkUPLC-Q-TOF MSQuEChERS

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