Determination of 27 Amino Acids in Sports Nutrition Food by Magnetic Dispersive Solid Phase Microextraction Coupled with UHPLC-Q-Orbitrap HRMS

HUANG Jia-le; CHEN Yang; DANG Hua; YAO Xiao-qing; HUANG Jia-yu

doi:10.12452/j.fxcsxb.23051802

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Determination of 27 Amino Acids in Sports Nutrition Food by Magnetic Dispersive Solid Phase Microextraction Coupled with UHPLC-Q-Orbitrap HRMS

Experimental Techniques and Methods | 更新时间：2024-03-13

- Determination of 27 Amino Acids in Sports Nutrition Food by Magnetic Dispersive Solid Phase Microextraction Coupled with UHPLC-Q-Orbitrap HRMS
- Journal of Instrumental Analysis Vol. 43, Issue 3, Pages: 455-463(2024)
- 作者机构：
  
  广州检验检测认证集团有限公司，广东广州 511447
- 作者简介：
- 基金信息：
- DOI：10.12452/j.fxcsxb.23051802
  CLC： O657.63;TS207.3
- Published：15 March 2024，
  
  Received：18 May 2023，
  
  Revised：21 December 2023，
- 稿件说明：
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黄嘉乐,陈扬,党华等.磁性分散固相微萃取/UHPLC-Q-Orbitrap HRMS测定运动营养食品中27种氨基酸[J].分析测试学报,2024,43(03):455-463.

HUANG Jia-le,CHEN Yang,DANG Hua,et al.Determination of 27 Amino Acids in Sports Nutrition Food by Magnetic Dispersive Solid Phase Microextraction Coupled with UHPLC-Q-Orbitrap HRMS[J].Journal of Instrumental Analysis,2024,43(03):455-463.
黄嘉乐,陈扬,党华等.磁性分散固相微萃取/UHPLC-Q-Orbitrap HRMS测定运动营养食品中27种氨基酸[J].分析测试学报,2024,43(03):455-463. DOI： 10.12452/j.fxcsxb.23051802.

HUANG Jia-le,CHEN Yang,DANG Hua,et al.Determination of 27 Amino Acids in Sports Nutrition Food by Magnetic Dispersive Solid Phase Microextraction Coupled with UHPLC-Q-Orbitrap HRMS[J].Journal of Instrumental Analysis,2024,43(03):455-463. DOI： 10.12452/j.fxcsxb.23051802.

摘要

基于磁性分散固相微萃取净化，建立了测定运动营养食品中27种氨基酸含量的超高效液相色谱-四极杆-静电场轨道阱高分辨质谱法。通过优化液相色谱条件、质谱条件和样品前处理过程，在20 min内实现了对27种目标物的测定。样品经涡旋振荡，超声提取，磁性氧化石墨烯分散固相微萃取净化，采用Thermo Accucore HILIC色谱柱分离，以0.1%甲酸水溶液（含5.0 mmol/L甲酸铵）和0.1%甲酸乙腈（含5.0 mmol/L甲酸铵）为流动相进行梯度洗脱，静电场轨道阱高分辨质谱检测，外标法定量。结果表明，27种目标化合物在一定质量浓度范围内线性良好，相关系数（

）均大于0.99，方法的定量下限为0.10~0.25 mg/kg，平均回收率为70.0%~93.0%，日内相对标准偏差（RSD，

=6）为1.6%~10%，日间RSD（

=5）为1.4%~5.2%。该方法高效灵敏，准确可靠，适用于运动营养食品中27种氨基酸的测定。

Abstract

A method for determination of 27 amino acids in sports nutrition foods was established based on magnetic dispersive solid phase microextraction purification，coupled with ultra-high performance liquid chromatography-quadrupole-orbitrap high-resolution mass spectrometry（UHPLC-Q-Orbitrap HRMS）. Through optimization of the liquid chromatography conditions，mass spectrometry conditions，and sample pretreatment process，analysis and determination of 27 target analytes were achieved within 20 minutes. The sample was subjected to vortex oscillation，ultrasonic extraction，dispersive solid phase microextraction purification with magnetic graphene oxide.The analytes were separated by a Thermo Accucore HILIC chromatographic column，and eluted with a gradient of 0.1% formic acid water solution containing 5.0 mmol/L formic acid ammonium and 0.1% formic acid acetonitrile containing 5.0 mmol/L formic acid ammonium as the mobile phase，followed by electrostatic trap high-resolution mass spectrometry detection. The results showed that the 27 target compounds had good linear correlations within a certain mass concentration range with correlation coefficients（

） greater than 0.99，and the quantitation limits of the method were 0.10-0.25 mg/kg，with recoveries ranged of 70.0%-93.0%. The intra-day relative standard deviations（RSDs，

=6） ranged of 1.6%-10%，and the inter-day RSDs（

=5） ranged of 1.4%-5.2%. The analysis method is highly efficient，sensitive，accurate and reliable，and is suitable for the determination of 27 amino acids in sports nutrition foods.

关键词

超高效液相色谱-四极杆-静电场轨道阱高分辨质谱磁性氧化石墨烯磁性分散固相微萃取运动营养食品氨基酸

Keywords

ultra-high performance liquid chromatography-quadrupole-orbitrap high-resolution mass spectrometrymagnetic graphene oxidemagnetic dispersive solid phase microextractionsports nutrition foodamino acids

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