The Need for Speed in Metabolomics: UHPLC with maXis UHR-Q-TOF-MS Analysis of Tea Extracts
By Aiko Barsch, Gabriela Zurek, Wiebke Lohmann, Bruker Daltonik GmbH, Bremen, Germany, Bruker

An untargeted metabolic profiling experiment of different black and green tea extracts was carried out using an UHPLC and maXis ESI-TOF-MS analytical system. Processed data was submitted to principal component analysis (PCA) to identify compounds discriminating the tea varieties. The compounds’ sum formulae were queried in public databases enabling the identification of compounds characteristic for green and black tea.

Iodide and Iodate in Seawater and Table Salt
By Deanna Hurum, Dionex Corporation

Iodide and iodate are important bio-available forms of the element iodine, an essential nutrient for aquatic life and humans. This AN describes how to determine iodide and iodate in samples with high salt concentrations.

Bile Acid Purification in Drug Discovery
By Scott Anderson and David Crowshaw, Grace Davison Discovery Sciences

Bile acids, such as Cholic acid are starting materials for the semi-synthesis of other medicinal steroids due to their availability as raw materials. Conjugation of cholic acid with glycine or taurine increases its water solubility for drug development. Using the RevealX™ technology of the Reveleris® iES flash chromatography system and the Reveleris® reversed-phase cartridge, chromophoric and non-chromophoric target compounds can be separated and isolated, in the presence of small impurities present, in a chemical reaction by a single chromatography run.

Quantitative Analysis of Carbonyl-DNPH Derivatives by UHPLC/UV
By Terry Zhang, Guifeng Jiang, Thermo Fisher Scientific

A fast, accurate and robust method for the separation and quantitation of parts per billion (ppb) concentrations of low molecular weight carbonyls using UHPLC/UV was developed was developed using the Thermo Scientific Accela 1250 UHPLC system.

Analysis of Water-Soluble Polymers Using Linear SEC Columns
By R. Roemling, Tosoh Bioscience

Water-soluble polymers are used in varoius applications. Their molecular weight distribution is usually characterized by size exclusion chromatography (SEC). This application describes the analysis of water-soluble polymers with a new generation of linear, polymer-based, semi-micro SEC columns using the EcoSEC SEC system.

Synthesis of a Bradykinin Analog using AmphiSpheres™ Resins
By Andrew Coffey, Varian, Inc

Bradykinin levels are increased as a result of the action of many ACE inhibitors, causing a reduction in blood pressure due to its role as a vasodilator. AmphiSpheres are very effective for the synthesis of bradykinin analogs.

Synthesis of HIV-1 gp41 using AmphiSpheres™ Resin
By Andrew Coffey, Varian, Inc

The 28 residue HIV-1 gp41 ectodomain sequence is difficult to synthesize. AmphiSpheres resins improve synthesis of “difficult” peptide sequences.

Analysis of Intact Lipids from Biologics Matrices by UPLC/High Definition MS
By John Shockcor, Hayley Crowe, Kate Yu, Henry Shion, Waters Corporation

The Waters ACQUITY UPLC System and SYNAPT G2 ion mobility MS is an ideal platform for the analysis of lipids. The method described is simple, effective, and yields rapid results with best-in-class resolution and sensitivity.

Analytical HPLC to Preparative HPLC: Scale-Up Techniques using a Natural Product Extract
Andrew Aubin and Ronan Cleary, Waters Corporation

This application note demonstrates that analytical chromatography can be successfully scaled to preparatory chromatography easily by using a systematic approach. Also demonstrated is the unique capability of the Waters AutoPurification System, which allows users to perform both analytical and preparatory chromatography on the same system with no performance compromise.

Analysis of Biomolecules by Size-Exclusion UltraPerformance Liquid Chromatography
Kenneth J. Fountain, Paula Hong, Susan Serpa, Edouard S. P. Bouvier, Damian Morrison, Waters Corporation

This application note will demonstrate the use of the new ACQUITY UPLC SEC solution for the improved detection and/or faster analysis of protein aggregates in biopharmaceuticals.

Bottle-brush polymers
Yan Xia and Robert H Grubbss, Wyatt Technology

Bottle-brush polymers are a type of high molecular weight (MW) graft polymers with very dense and regularly-spaced side chains.

With the introduction of Antec’s ROXY™ EC system, the synthesis of metabolites as well as the mimicking of phase I and II metabolism has become possible in routine within a few minutes.

The analysis of urine for drugs of abuse via chromatographic methods is commonplace but can be complicated by high matrix effects and frequent co-elution. Novel time-of-flight mass spectrometry in combination with sophisticated deconvolution software was tested and found to provide increased confidence in results due to the high sensitivity and quality of spectra achieved.

This application note describes how to extract the surfactant alkylbenzene sulfonate, a common household detergent, from up to 5 mL of sample by online SPE using a polymeric reversed-phase column. This is followed by releasing the extracted surfactant to determine it using fluorescence detection.

To meet the growing demand for determining both 25-mono-hydroxy- Vitamin D2 and Vitamin D3 in one run, a fully automated method has been created, combining on-line SPE and LC-MS in one integrated system (Symbiosis™ Pico). This method requires no manual pretreatment step(s) anymore, just one operator step is required before SPE and LC-MS are executed fully automated in one unattended run. This results in high throughput, low CV’s and high precision.