Hydrophilic interaction ultra-performance liquid chromatography coupled with triple-quadrupole tandem mass spectrometry for highly rapid and sensitive analysis of underivatized amino acids in functional foods

Zhou, Guisheng; Pang, Haijun; Tang, Yuping; Yao, Xin; Mo, Xuan; Zhu, Shaoqing; Guo, Sheng; Qian, Dawei; Qian, Yuqing; Su, Shulan; Zhang, Li; Jin, Chun Hua; Qin, Yong; Duan, Jin‐Ao

doi:10.1007/s00726-013-1463-7

Cited by 55 publications

(31 citation statements)

References 34 publications

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“…HPLC-MS/MS appeared reasonably fast (5 -15 min) but LOD were still too high [31] [32]. Similar conditions (10 min, LOD > 10 nM) were obtained by Zhou et al [33] who used UPLC with a triple quadrupole and a specific column. Elsewhere it has been reported that retention times and thus the response signal of underivatized amino acids could be improved on classic C 18 column by an ion-pairing agent [34]- [36].…”

Section: Introductionsupporting

confidence: 67%

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A Method for Detection of Trace Concentrations of Underivatized Amino Acid in Hydrothermal Fluids by Ion-Pairing Reversed-Phase UPLC-ESI-QTOF-MS

Konn

Magnér²,

Charlou³

et al. 2015

AJAC

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Investigation of amino acids in hydrothermal systems is of prime importance for the understanding of geochemistry and microbiology of hydrothermal vents and plumes, for carbon and metals global cycles, for metabolism of some hydrothermal microorganisms and for the origin of life issue. Extensive theoretical and experimental work on amino acids behaviour in hydrothermal fluids has been done, conversely only few data exist on natural samples. Because each hydrothermal vent is unique, the more data we collect the better we will be able to address each of these questions. Usually amino acids in hydrothermal fluids have been measured by HPLC-FLD. The chromatographic separation was at least 26 min and up to 135 min and the required derivatization step may be time consuming, may use harmful chemicals and may be source of contamination. Alternatively, we describe here a method combining quickness (4.5 min), high resolution (10,000), very low LOD (sub-ppb) and without derivatization. Characterisation and separation of 10 relevant proteinogenic underivatized amino acids was achieved by ion-pairing reversed-phase Ultrahigh Performance Liquid Chromatography-Electrospray Ionisation-Quadrupole Time of Flight-Mass Spectrometry (UPLC-ESI-QTOF-MS). Excellent linearity in the response was obtained for all amino acids with correlation coefficients > 0.9921. This method was successfully applied to natural hydrothermal fluid samples from ultramafic-hosted vents of the Mid-Atlantic Ridge region. Results are consistent with the only 2 other studies published on ultramafic-hosted vents and complete the few available data.

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Section: Introductionsupporting

confidence: 67%

“…Separation was achieved in less than 4.5 min with very nice peak shapes (Figure 1); being about 3 times faster than with HPLC which is a common feature [35] [51]- [53]. This is also faster than other work using UPLC [33] [39] [40].…”

Section: Chromatography and Separationmentioning

confidence: 89%

A Method for Detection of Trace Concentrations of Underivatized Amino Acid in Hydrothermal Fluids by Ion-Pairing Reversed-Phase UPLC-ESI-QTOF-MS

Konn

Magnér²,

Charlou³

et al. 2015

AJAC

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“…Prior to DoE, 22 LC solvent systems were compared using the standard mix. These solvents were based on a literature search and are listed in Table S4 (Want et al 2010; Kivilompolo et al 2013; Ivanisevic et al 2013; Zhou et al 2013). Mass spectrometry settings were based on data from the ion-switching method development, where desolvation temperature and gas flow were set to 500°C and 1000L/Hr respectively.…”

Section: Methodsmentioning

confidence: 99%

Comprehensive optimization of LC–MS metabolomics methods using design of experiments (COLMeD)

Rhoades

Weljie

2016

Metabolomics

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Introduction Both reverse-phase and HILIC chemistries are deployed for liquid-chromatography mass spectrometry (LC-MS) metabolomics analyses, however HILIC methods lag behind reverse-phase methods in reproducibility and versatility. Comprehensive metabolomics analysis is additionally complicated by the physiochemical diversity of metabolites and array of tunable analytical parameters. Objective Our aim was to rationally and efficiently design complementary HILIC-based polar metabolomics methods on multiple instruments using Design of Experiments (DoE). Methods We iteratively tuned LC and MS conditions on ion-switching triple quadrupole (QqQ) and quadrupole-time-of-flight (qTOF) mass spectrometers through multiple rounds of a workflow we term COLMeD (Comprehensive optimization of LC-MS metabolomics methods using design of experiments). Multivariate statistical analysis guided our decision process in the method optimizations. Results LC-MS/MS tuning for the QqQ method on serum metabolites yielded a median response increase of 161.5% (p<0.0001) over initial conditions with a 13.3% increase in metabolite coverage. The COLMeD output was benchmarked against two widely used polar metabolomics methods, demonstrating total ion current increases of 105.8% and 57.3%, with median metabolite response increases of 106.1% and 10.3% (p<0.0001 and p<0.05 respectively). For our optimized qTOF method, 22 solvent systems were compared on a standard mix of physiochemically diverse metabolites, followed by COLMeD optimization, yielding a median 29.8% response increase (p<0.0001) over initial conditions. Conclusions The COLMeD process elucidated response tradeoffs, facilitating improved chromatography and MS response without compromising separation of isobars. COLMeD is efficient, requiring no more than 20 injections in a given DoE round, and flexible, capable of class-specific optimization as demonstrated through acylcarnitine optimization within the QqQ method.

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“…Despite increasing the time and effort required for sample preparation, chemical derivatization makes amino acid assignment and quantitation down to the μM level amenable to routine analysis. Additional LC/MS methods for the detection of underivatized amino acids have been described that rely on 12 to 15 min analytical times and multiple reaction monitoring (MRM) for amino acid detection ((Thiele et al 2012; Zhou et al 2013; Yao et al 2013; Buiarelli et al 2013; Le et al 2014)).…”

Section: Introductionmentioning

confidence: 99%

Three-minute method for amino acid analysis by UHPLC and high-resolution quadrupole orbitrap mass spectrometry

2015

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Amino acid analysis is a powerful bioanalytical technique for many biomedical research endeavors, including cancer, emergency medicine, nutrition and neuroscience research. In the present study, we present a three minute analytical method for underivatized amino acid analysis that employs ultra-high performance liquid chromatography and high resolution quadrupole orbitrap mass spectrometry. This method has demonstrated linearity (mM to nM range), reproducibility (intra-day<5%, inter-day<20%), sensitivity (low fmol) and selectivity. Here, we illustrate the rapidity and accuracy of the method through comparison with conventional liquid chromatography-mass spectrometry methods. We further demonstrate the robustness and sensitivity of this method on a diverse range of biological matrices. Using this method we were able to selectively discriminate murine pancreatic cancer cells with and without knocked down expression of Hypoxia Inducible Factor 1α; plasma, lymph and bronchioalveolar lavage fluid samples from control versus hemorrhaged rats; and muscle tissue samples harvested from rats subjected to both low fat and high fat diets. Furthermore, we were able to exploit the sensitivity of the method to detect and quantify the release of glutamate from sparsely isolated murine taste buds. Spiked in light or heavy standards (13C6-arginine, 13C6-lysine, 13C515N2-glutamine) or xenometabolites were used to determine coefficient of variations, confirm linearity of relative quantitation in four different matrices, and overcome matrix effects for absolute quantitation. The presented method enables high-throughput analysis of low abundance samples requiring only one percent of the material extracted from 100,000 cells, 10 μl of biological fluid, or 2 mg of muscle tissue.

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Hydrophilic interaction ultra-performance liquid chromatography coupled with triple-quadrupole tandem mass spectrometry for highly rapid and sensitive analysis of underivatized amino acids in functional foods

Cited by 55 publications

References 34 publications

A Method for Detection of Trace Concentrations of Underivatized Amino Acid in Hydrothermal Fluids by Ion-Pairing Reversed-Phase UPLC-ESI-QTOF-MS

A Method for Detection of Trace Concentrations of Underivatized Amino Acid in Hydrothermal Fluids by Ion-Pairing Reversed-Phase UPLC-ESI-QTOF-MS

Comprehensive optimization of LC–MS metabolomics methods using design of experiments (COLMeD)

Three-minute method for amino acid analysis by UHPLC and high-resolution quadrupole orbitrap mass spectrometry

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