Integration of solid phase extraction with HILIC-MS/MS for analysis of free amino acids in source water

Qiu, Junlang; Craven, Caley B.; Wawryk, Nicholas J.P.; Carroll, Kristin; Li, Xing‐Fang

doi:10.1016/j.jes.2022.04.025

Cited by 8 publications

(7 citation statements)

References 40 publications

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Section: Resultsmentioning

confidence: 99%

“…The accurate quantitative determination of AAs has been a long historical project with continuous improvements and innovations have been achieved. Several publications have reported AA analysis in foods and biological fluids using GC–MS, capillary electrophoresis, HILIC-MS/MS, ion-paired LC–MS/MS, electrochemical detection (CE), ion exchange chromatography, and HPLC. , Most of these methods depend on pre- or postcolumn derivatization to improve the detection sensitivity. However, elimination of derivatization steps attracts many researchers, and many studies have described the analysis of AAs without derivatization steps such as underivatized determination of free AAs in honey using LC–MS/MS, branched-chain AAs in maple syrup urine disease using LC–MS/MS, evaluation embryo viability using CE-MS, urine analysis by LC–MS/MS, ion exchange, CE-MS coupled to a porous layer-gold nanoparticle-modified chiral column, AAs and peptides in nutritive mixtures in the total parenteral nutrition solution, and online coupling of UV, fluorescence, and electrochemical detection .…”

Section: Resultsmentioning

confidence: 99%

See 1 more Smart Citation

Underivatized Amino Acid Chromatographic Separation: Optimized Conditions for HPLC-UV Simultaneous Quantification of Isoleucine, Leucine, Lysine, Threonine, Histidine, Valine, Methionine, Phenylalanine, Tryptophan, and Tyrosine in Dietary Supplements

2022

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Amino acids (AAs) are considered as the building blocks of life. Unlike nonessential AAs, the human body cannot synthesize essential AAs and should be supplied in food or dietary supplements. The aim of the work is simultaneous HPLC-UV determination of 10 structurally related AAs without pre- or postderivatization in powdered dietary supplements (PDSs). This was challenging, especially because PDS has no standardized procedures for its quality control. HPLC-UV chromatograms of the 10 AAs were recorded using a gradient elution of the mobile phase on a CLC-C18 column at 225 nm. The elution started with 100% of phosphate buffer (pH 7.4, 10 mM) for 10 min; then, the concentration of acetonitrile increased linearly to reach 50% for another 15 min at room temperature. Good separation was achieved within a 25 min run time without pre- or postderivatization. The method was carefully validated according to the ICH guidelines over the linearity range of 100–200, 50–200, 20–150, 50–400, 20–250, 75–175, 50–250, 50–250, 50–300, and 5–100 μg/mL for l -lysine, l -threonine, l -histidine, l -valine, l -methionine, l -isoleucine, l -leucine, l -tyrosine, l -phenylalanine, and l -tryptophan, respectively, with mean recoveries ranges between 98.91 and 100.77. The method was found to be precise, and the relative standard deviation (RSD) was found to be between 0.28 and 1.92 with recoveries between 97.91 and 101.11. The method was found to be robust that resists deliberate changes in pH, flow rate, and mobile-phase percentages. It was successfully applied for the analysis of PDSs. The proposed method could be very useful for the quality control of the 10 structurally related AAs during their synthesis and for testing raw materials and pharmaceutical preparations.

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Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Underivatized Amino Acid Chromatographic Separation: Optimized Conditions for HPLC-UV Simultaneous Quantification of Isoleucine, Leucine, Lysine, Threonine, Histidine, Valine, Methionine, Phenylalanine, Tryptophan, and Tyrosine in Dietary Supplements

2022

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“…Triplicate 500 mL aliquots of source water samples were extracted by SPE using the same procedures previously reported . Briefly, each sample (500 mL) was first prepared with addition of 2 mL of an aqueous ammonium hydroxide solution (30 wt %).…”

Section: Methodsmentioning

confidence: 99%

“…Triplicate 500 mL aliquots of source water samples were extracted by SPE using the same procedures previously reported. 43 Briefly, each sample (500 mL) was first prepared with addition of 2 mL of an aqueous ammonium hydroxide solution (30 wt %). Oasis MAX cartridges (6 cc, 150 mg) were preconditioned with methanol (2 mL), followed by an aqueous ammonium hydroxide solution (4 mL, 0.5 wt %).…”

Section: ■ Introductionmentioning

confidence: 99%

Amino Acids as Potential Precursors to Odorous Compounds in Tap Water during Spring Runoff Events

Craven

Wawryk

Carroll

et al. 2023

Environ. Sci. Technol.

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The onset of spring runoff in northern climates and tap water odor events are difficult to predict because common water quality parameters cannot fully explain the intermittent odor events that occurred over past decades. Studies have shown that small polar water-soluble compounds, such as amino acids (AAs), leach first from ice/snowmelt. AAs are known to produce odorous compounds, such as aldehydes and chloroaldimines, upon chlorination. Therefore, we proposed that AAs may serve as markers for small and soluble organics that contribute to the odor of chlorinated tap water. Here, we studied the occurrence of AAs in source water collected at two water treatment plants and the odor profiles of tap water at >300 homes during the 2021 and 2022 spring runoff events. AA concentrations were at baseline levels (<100 ng/L) during the 2021 runoff but much higher (up to 5500 ng/ L) in 2022 and associated with an escalation in odor complaints. AA concentrations peaked at the onset of the 2022 spring runoff and corresponded with the strongest reported odor intensities in tap water. We obtained high resolution MS and MS/MS spectra of chloroaldimines and confirmed the formation of chloroaldimines under chlorination of the six AAs detected in source water. The results indicate that AAs signal the onset of spring runoff and represent small polar water-soluble compounds that may contribute to tap water odor problems.

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“…In the determination of 23 AAs in exhaled breath condensate samples from pediatric leukemia patients, the AAs could be better separated using vacuum evaporation concentration than the lyophilization method [163]. In determining environmental water samples, SPE-treated samples had less matrix effects than the large-volume injection method [164]. In addition, to reduce the impact of matrix effects and other sources of error in the preparation of the sample, quadruple isotope dilution strategies methods have been widely used to determine free AAs in plasma and urine [165].…”

Section: 14mentioning

confidence: 99%

Overview of chromatographic and electrophoretic methods for the determination of branched‐chain amino acids

Yin

Adams

Schepdael

2023

J of Separation Science

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The significance of branched‐chain amino acids in diseases was clearly shown over the years. This review aims to describe the available techniques for their analytical determination. The article provides examples of the use of various analytical methods. The methods are divided into two categories: derivatization and non‐derivatization approaches. Separation is achieved through different chromatography or capillary electrophoresis techniques and can be combined with different detectors such as flame ionization, ultraviolet, fluorescence, and mass spectrometry. It compares the application of various derivatization reagents or detection as such for different detectors.

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Integration of solid phase extraction with HILIC-MS/MS for analysis of free amino acids in source water

Cited by 8 publications

References 40 publications

Underivatized Amino Acid Chromatographic Separation: Optimized Conditions for HPLC-UV Simultaneous Quantification of Isoleucine, Leucine, Lysine, Threonine, Histidine, Valine, Methionine, Phenylalanine, Tryptophan, and Tyrosine in Dietary Supplements

Underivatized Amino Acid Chromatographic Separation: Optimized Conditions for HPLC-UV Simultaneous Quantification of Isoleucine, Leucine, Lysine, Threonine, Histidine, Valine, Methionine, Phenylalanine, Tryptophan, and Tyrosine in Dietary Supplements

Amino Acids as Potential Precursors to Odorous Compounds in Tap Water during Spring Runoff Events

Overview of chromatographic and electrophoretic methods for the determination of branched‐chain amino acids

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