Liquid chromatography-mass spectrometry method for isomer separation and detection of sugars, phophorylated sugars and organic acids v1

2022 ◽  
Author(s):  
Somnath Koley ◽  
Kevin L. Chu ◽  
Saba S. Gill ◽  
Doug K. Allen
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Standard Operating Procedure ◽  
Central Carbon Metabolism ◽  
Exchange Chromatography ◽  
Isomer Separation ◽  
Enhanced Sensitivity ◽  
Wide Range ◽  
Phosphorylated Sugars ◽  
Liquid Chromatographic

This standard operating procedure is used to achieve effective separation of a wide range of polar metabolites found in central carbon metabolism via a hybrid liquid chromatographic method (ion-exchange chromatography and hydrophilic interaction liquid chromatography (HILIC)) using an Intrada Organic Acid column (Imtakt) coupled with triple quadrupole mass spectrometry. This method gives improved resolution while showing enhanced sensitivity for the detection of low abundance phosphorylated sugars compared with standard HILIC methods.

Developments in mycotoxin analysis: an update for 2012-2013

2014 ◽  
Vol 7 (1) ◽  
pp. 3-33 ◽  
Author(s):  
F. Berthiller ◽  
P.A. Burdaspal ◽  
C. Crews ◽  
M.H. Iha ◽  
R. Krska ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Sample Preparation ◽  
Ergot Alkaloids ◽  
Tandem Mass ◽  
Wide Range ◽  
Rapid Spread ◽  
Food And Feed ◽  
Mycotoxin Analysis ◽  
The Individual

This review highlights developments in mycotoxin analysis and sampling over a period between mid-2012 and mid-2013. It covers the major mycotoxins: aflatoxins, Alternaria toxins, ergot alkaloids, fumonisins, ochratoxins, patulin, trichothecenes and zearalenone. A wide range of analytical methods for mycotoxin determination in food and feed were developed last year, in particular immunochemical methods and liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS)-based methods. After a section on sampling and sample preparation, due to the rapid spread and developments in the field of LC-MS/MS multimycotoxin methods, a separate section has been devoted to this area of research. It is followed by a section on mycotoxins in botanicals and spices, before continuing with the format of previous reviews in this series with dedicated sections on method developments for the individual mycotoxins.

Gas Chromatographic and Gas Chromatographic-Mass Spectrometric Confirmation of 2,4- and 2,6-Toluenediamine Determined by Liquid Chromatography in Aqueous Extracts

1982 ◽  
Vol 65 (6) ◽  
pp. 1388-1394 ◽  
Author(s):  
Roger C Snyder ◽  
William C Brumley ◽  
Charles V Breder ◽  
Thomas Fazio
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Mass Spectrometric ◽  
Gas Liquid Chromatography ◽  
Aqueous Extracts ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic ◽  
Chromatographic Mass

Abstract The confirmation of 2,4- and 2,6-toluenediamine (TDA) in aqueous extracts from boil-in-bags and retortable pouches is described. The extracts were initially analyzed by a high performance liquid chromatographic procedure and any apparent 2,4- and/or 2,6-TDA were quantitated. The liquid chromatographic effluent corresponding to any apparent 2,4- or 2,6-TDA was collected. TDA was then partitioned into ethyl acetate and reacted with trifluoroacetic anhydride (TFAA). The TDA-TFAA derivative formed was confirmed by gas-liquid chromatography (GLC) using a 1.2 m × 0.32 cm nickel column packed with 6% OV-17 on Superpak-20M. Results obtained from analyzing extracts of several retortable pouches and boil-in-bags showed levels of TDA migration ranging from <0.1 to 2.2 ppb (μg/L). Additional confirmation of the TDA-TFAA derivative from retortable pouches by multiple ion detection GC/mass spectrometry is also described.

scholarly journals Transfer of a Multiclass Method for over 60 Antibiotics in Food from High Resolution to Low Resolution Mass Spectrometry

Molecules ◽  
2019 ◽  
Vol 24 (16) ◽  
pp. 2935 ◽  
Author(s):  
Giusepponi ◽  
Paoletti ◽  
Barola ◽  
Moretti ◽  
Saluti ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
High Resolution ◽  
Development Process ◽  
Tandem Mass ◽  
Laboratory Studies ◽  
Low Resolution ◽  
Method Transfer ◽  
Wide Range ◽  
Microbial Residues

A multiclass method has been developed to screen and confirm a wide range of anti-microbial residues in muscle and milk, and validated using liquid-chromatography coupled to (low-resolution, LR) tandem mass spectrometry (LC-QqQ). Over sixty antibiotics, belonging to ten distinct families, were included in the method scope. The development process was rapidly concluded as a result of two previously implemented methods. This consisted of identical sample treatments, followed by liquid chromatography, and coupled with high-resolution (HR) mass spectrometry (LC-Q-Orbitrap). The validation study was performed in the range between 10–1500 μg·kg−1 for muscles and 2–333 μg·kg−1 for milk. The main performance characteristics were estimated and, then, compared to those previously obtained with HR technique. The validity of the method transfer was ascertained also through inter-laboratory studies.

scholarly journals A gas-liquid-chromatographic procedure for separating a wide range of metabolites occurring in urine or tissue extracts

1966 ◽  
Vol 101 (3) ◽  
pp. 792-810 ◽  
Author(s):  
CE Dalgliesh ◽  
EC Horning ◽  
MG Horning ◽  
KL Knox ◽  
K Yarger
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Shikimic Acid ◽  
Methyl Esters ◽  
Peak Position ◽  
Gas Chromatography Mass Spectrometry ◽  
Tissue Extracts ◽  
Wide Range ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic

1. A gas-liquid-chromatographic procedure is described which permits separation and identification on the same chromatogram of a wide range of substances occurring in urine or tissue extracts. The method uses hydrogen flame ionization, which detects organic compounds whether free or conjugated with no requirement for specific reactive groups. 2. For chromatography, carboxyl groups are quantitatively converted into methyl esters or trimethylsilyl esters. Phenolic, alcoholic and potential enolic groups are converted into trimethylsilyl ethers. Separations are carried out on a 6ft. column of either 10% F-60 (a polysiloxane) or 1% F-60, temperature programming at 2 degrees /min. being used over such part of the temperature range 30 degrees -260 degrees as is required. Propionyl derivatives of hydroxy compounds can also be used, but only on a non-quantitative basis. Derivatives and columns have been selected for optimum range of usefulness when large numbers of samples are examined by using automated gas chromatography. 3. The method is applicable to: fatty acids above butyric acid; di- and tri-carboxylic acids; hydroxy acids and keto acids; polyhydroxy and alicyclic compounds such as glycerol, inositol, quinic acid, shikimic acid, ascorbic acid and sugar alcohols; aromatic hydroxy and acidic compounds, both benzenoid and indolic; sesquiterpenes; steroids; glycine conjugates; mercapturic acids; glucuronides. It is not satisfactory for sulphate conjugates, iminazoles or polypeptides. 4. Methylene units provide an accurate and reproducible parameter for characterizing peak position. Methylene unit values are reported for a large variety of substances occurring in, or related to those occurring in, urine and tissue extracts. 5. The nature of derivatives was confirmed by combining gas chromatography with mass spectrometry. Combined gas chromatography-mass spectrometry gives a diagnostic tool of great power in the evaluation of metabolic patterns, and various uses are discussed.

Comparison of different anion-exchange chromatography resins for the purification of cyanobacterial microcystins

2015 ◽  
Vol 16 (1) ◽  
pp. 1-8 ◽  
Author(s):  
Theerasak Somdee ◽  
Anchana Somdee
Keyword(s):  
Liquid Chromatography ◽  
Anion Exchange ◽  
High Performance ◽  
Total Yield ◽  
Deae Cellulose ◽  
Anion Exchange Chromatography ◽  
Exchange Chromatography ◽  
Ionization Mass ◽  
Freeze Dried ◽  
Wide Range

For the first time, different types of diethylaminoethyl (DEAE) anion-exchange resins, widely used in previous studies, were investigated to determine the most effective resin for the purification of microcystins (MCs). MCs were extracted from freeze-dried Microcystis aeruginosa cells that had been harvested from the Bueng Nong Khot reservoir, Khon Kaen, Thailand. The toxins were precipitated with ammonium sulfate and then fractionated using five different anion-exchange chromatography resins, followed by chromatography with a C18 cartridge. The toxins were further identified via liquid chromatography–electrospray ionization–mass spectrometry (LC-ESI-MS) analysis, and the yields and purity were determined by high-performance liquid chromatography (HPLC) with ultraviolet detection. DEAE Sephadex A-25 exhibited the best overall performance for MC purification regarding both yield and purity, followed by DEAE cellulose, DEAE Sephacel, DEAE Sepharose Fast Flow and Toyopearl DEAE. Four MC variants, MC-RR, MC-FR, [Dha7]MC-LR and MC-WR, were obtained, and [Dha7]MC-LR was the major variant, with a total yield of 53.08 mg and a purity of 95% using the Sephadex resin. This study indicates that protein precipitation and single-column chromatography using DEAE Sephadex A-25 constitute an effective method for the purification of a wide range of MC variants.

scholarly journals A comparison of one-dimensional and microscale two-dimensional liquid chromatographic approaches coupled to high resolution mass spectrometry for the analysis of complex samples

2015 ◽  
Vol 7 (18) ◽  
pp. 7697-7706 ◽  
Author(s):  
Juri Leonhardt ◽  
Thorsten Teutenberg ◽  
Jochen Tuerk ◽  
Michael P. Schlüsener ◽  
Thomas A. Ternes ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
High Resolution ◽  
High Resolution Mass Spectrometry ◽  
Two Dimensional ◽  
Complex Samples ◽  
One Dimensional ◽  
Open Questions ◽  
Liquid Chromatographic ◽  
Resolution Mass

The interest in two-dimensional liquid chromatography separations is growing every year together with the number of open questions on the benefits.

Quantitation of Radio-Labelled Vitamin K1 and Vitamin K1 Epoxide in Plasma by High Pressure Liquid Chromatography

1978 ◽  
Vol 39 (02) ◽  
pp. 466-473 ◽  
Author(s):  
Thorir D Bjornsson ◽  
Sarah E Swezey ◽  
Peter J Meffin ◽  
Terrence F Blaschke
Keyword(s):  
High Pressure ◽  
Liquid Chromatography ◽  
Coefficient Of Variation ◽  
Chromatographic Method ◽  
Vitamin K1 ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatographic Method ◽  
Wide Range ◽  
Liquid Chromatographic

SummaryA convenient, accurate and reproducible high pressure liquid chromatographic method for the quantitation of radio-labelled vitamin K1 and vitamin K1 epoxide in plasma is described. The method involves the determination of total ether extractable radioactivity, and a chromatographic separation to determine the relative quantities of radio-labelled vitamin K1 and vitamin K1 epoxide. The method is useful over a wide range of ratios of the two compounds, and has a coefficient of variation of approximately 5%.

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