The Application Notebook-06-01-2012

The Application Notebook

Lowering Detection Limits for 1,4-Dioxane in Drinking Water Using Large Volume Injection in an Unmodified Splitless GC Inlet

June 01, 2012

Environmental

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Concurrent solvent recondensation–large volume splitless injection (CSR-LVSI), an alternative to programmed temperature vaporization (PTV), typically requires a special GC inlet. The technique described here uses an unmodified split/splitless inlet with CSR-LVSI to lower detection limits for the analysis of 1,4-dioxane in drinking water.

Enhanced Results of Diesel Range Organics Analysis with High-Temperature Gas Enhanced Chromatography

June 01, 2012

Environmental

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Diesel range organic (DRO) compounds have boiling points similar to diesel fuel (C10–C28), ranging from 170–430 ?C. These heavy compounds are amenable to GC-FID analysis; however, important considerations should be taken to ensure reproducible results over repeated injections.

The Analysis of 1,4-Dioxane for EPA Method 522 and UCMR 3

June 01, 2012

Environmental

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This application note will demonstrate the extraction of 1,4-dioxane from an aqueous matrix using option 1 of EPA Method 522 for 500 mL initial volume sample. It will make use of the SmartPrep Cartridge Extraction system to produce a valid initial demonstration of precision (IDP) and initial demonstration of accuracy (IDA).

Characterization of Polymeric Excipients by SEC-IR

June 01, 2012

Pharmaceutical/Drug Discovery

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Excipients are pharmacologically inactive substances used as carrier and release controllers for active drug ingredients. A significant amount (30–80% solid) of polymeric excipients such as hydroxyl propyl cellulose (HPC), hydroxypropyl methyl cellulose (HPMC), hydroxypropyl methyl cellulose acetate succinate (HPMCAS), and povidone are used.

Rapid LC–MS-MS Analysis of Heterocyclic Amines in Salmon

June 01, 2012

Food & Beverage

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Heterocyclic amines (HCAs) are a class of compounds that are formed when amino acids from meat proteins react with glucose and creatine under high-temperatures, as is associated with frying or grilling over an open flame (1–3). Studies have correlated the consumption of high levels of HCAs with an increased risk of some forms of cancer.

Detection of Protein Heterogeneity by HPLC

June 01, 2012

Pharmaceutical/Drug Discovery

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Protein heterogeneity is generated by post-translational modification, decomposition, and a variety of other processes, including chemical modification, denaturation, and aggregation. Since antibodies and recombinant proteins are now widely used for therapeutic treatment, it is essential to evaluate their heterogeneity during development, stability testing, and in the quality control of the final product.

Analysis of "Broad Spectrum" UVA and UVB Components in Sun Care Products for Compliance with New FDA Regulations

June 01, 2012

General

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The FDA has made changes to how products containing sunscreen are labeled in the U.S. to ensure they meet the new regulations set forth for safety and effectiveness. The new regulations will require companies that want to use the "broad spectrum" label to test for both UVA and UVB protection.

UCMR 3 Low-Level VOC Analysis by Purge and Trap Concentration and GC-MS Using Selective Ion Monitoring

June 01, 2012

Environmental

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The United States Environmental Protection Agency (US EPA) has established the Unregulated Contaminant Monitoring Program to collect data for contaminants suspected to be present in drinking water (1). The US EPA is currently proposing Unregulated Contaminant Monitoring Rule 3 (UCMR 3) which will collect data from January 2013 through December 2015. Because of the impact on public health and safety, it is vital to have a system that can detect and analyze for these compounds at low levels.

The Characterization of Sugar Beet Pectin using the EcoSEC GPC System Coupled to Multi-Angle Light Scattering, Quasi-Elastic Light Scattering, and Differential Viscometry

June 01, 2012

Food & Beverage

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The need to increase the use of low valued co-products derived from the processing of sugar beets has prompted the investigation of the structure of the pectin extracted from sugar beet pulp. The characterization of sugar beet pectin is essential as it has the potential to be used in the production of industrial products, e.g., as an emulsifying agent in food systems.

Ascentis Express 5 micron: A Fused-Core Particle HPLC Column for Faster HPLC Separations with No Backpressure Concerns

June 01, 2012

General

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Ascentis Express 5 micron columns provide a new choice for improving the performance of traditional HPLC systems. Based on Fused-Core particle technology, Ascentis Express provides the benefits of high speed and high efficiencies without the concerns of smaller particle columns. Due to the high efficiencies at low backpressures, Ascentis Express 5 micron can benefit conventional HPLC users with no drawbacks.

Low Level PAH Detection with an Extensive Dynamic Range

June 01, 2012

Environmental

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The analysis of PAHs in less than 16 min using hydrogen as carrier gas and the PerkinElmer? Clarus? SQ 8 GC/MS operating in SIM mode is presented. Detection limits down to 0.5 pg on-column and a wide dynamic range are reported.

Analytical Methods to Characterize and Quantify PEG and PEGylated Biopharmaceuticals

June 01, 2012

Pharmaceutical/Drug Discovery

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Biotherapeutic peptides and proteins are often PEGylated (covalently bonded to polyethylene glycol polymers) to improve bioavailability, reduce immunogenicity, and extend circulating half-life (1). Achieving the desired properties for each application depends on optimizing the number and site of polymers attached, chain length, and the degree of chain branching.

Analysis of Antioxidants in Foods and Dietary Supplements using HPLC with Post-Column Derivatization.

June 01, 2012

Food & Beverage

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Antioxidants protect cells from the damaging effects of free radicals and offer numerous benefits for human health. Many phenolic compounds found in plants, as well as some vitamins, exhibit antioxidant activity. Several colorimetric assays exist to measure the total antioxidant capacity, typically expressed as Trolox or Gallic acid equivalents.

Lenses or No Lenses? A Study of Ion Transfer Efficiency at Interfaces in a Lens-Free Triple Quadrupole MS

June 01, 2012

General

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The efficiency of ion transfer between the quadrupole mass analyzers and the Q2 collision cell in a triple quadrupole mass spectrometry (MS) is critical for instrument robustness and sensitivity. Q2 is a radio frequency (RF) only non-mass filtering quadrupole containing only an inert collision gas such as Ar, He, or N2 to provide collision induced dissociation of the precursor ion selected in Q1.

Glycan Analysis using HPLC with Charged Aerosol Detection and MS Detectors

June 01, 2012

Medical/Biological

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Simple, rapid and accurate methods have been developed for the analysis of simple carbohydrates including mono- or disaccharides, or as fairly small glycans (6–11 residues) liberated from glycoproteins using charged aerosol detection combined with mass spectrometry techniques.

Molecular Weight Determination of Low-Molecular-Weight Heparins: SEC/MALS vs. SEC/UV-RI

June 01, 2012

Medical/Biological

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Low-molecular-weight heparins (LMWHs) are obtained by fractionation or depolymerization of natural heparins. They are defined as having a mass-average molecular weight of less than 8000 and for which at least 60% of the total weight has a molecular mass less than 8000.

Unique Effects of Two Mobile Phase Alcohols on the RegisPack CLA-1 Chiral Stationary Phase (CSP)

June 01, 2012

Chiral

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Typical chiral stationary phase (CSP) screening paradigms utilize a single alcohol component as co-solvent in its mobile phase. Recent unexpected observations have demonstrated that mixed-alcohol mobile phases can enhance or even introduce peak resolution when none existed in a mono-alcohol system.

Size-Exclusion Ultra Performance Liquid Chromatography Analysis of Insulin

June 01, 2012

Pharmaceutical/Drug Discovery

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Insulin was the first recombinant pharmaceutical produced. Currently, one of the critical quality control attributes of therapeutic insulin in the US and European Pharmacopoeia (USP and EP) monograph is the level of covalent high molecular weight (HMW) insulin as determined by HPLC size-exclusion chromatography.

Novel Malaria Vaccine Candidates

June 01, 2012

Pharmaceutical/Drug Discovery

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Malaria remains one of the world's most deadly diseases, killing a child under five years of age every 30 s. Our branch aims to produce and characterize recombinant protein vaccines for Phase I and II human trials.

Practical Advice for High Throughput Ion Exchange Separations using Non-porous Particles

June 01, 2012

Medical/Biological

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Ion exchange is a perfect technique for analyzing large biomolecules such as proteins, peptides and oligonucleotides. These complex compounds contain numerous components (amino acids, nucleotides, glycans etc.) many of which possess a charged side chain or backbone.

Effective Cleanup and Analysis of Metronidazole from Foaming Facial Cleanser

June 01, 2012

General

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When working with complex matrices such as personal care products, sample preparation is perhaps the most difficult step of the analysis process. By utilizing a targeted sample preparation technique, such as ion-exchange SPE, analysis can be significantly improved as compared to less targeted techniques such as liquid-liquid extraction.

The Scherzo Family Columns Simultaneously Separate Acidic and Basic Pharmaceutical Compounds and Resolve Better than a Standard C18 Column

June 01, 2012

Pharmaceutical/Drug Discovery

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Compounds such as ibuprofen, chlorpheniramine, and allantoin are important in the field of pharmaceuticals and cosmetics. The analysis of acidic and basic compounds is particularly important but it is sometimes difficult to analyze both acidic and basic compounds on a single standard C18 column. Imtakt's Scherzo SM-C18 and Scherzo SW-C18 HPLC columns can separate acidic ibuprofen and basic chlorpheniramine simultaneously.

Resistive Glass Inlet Tubes Increase Ion Throughput

June 01, 2012

General

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Resistive glass tubes and plates are designed to guide ions by generating a uniform electric field. Photonis resistive glass products are composed of a proprietary lead silicate glass that has been specially processed to create a resistive layer at the surface. The resistivity can be varied over several orders of magnitude to suit the specific application.

Rapid Sampling and Identification of Volatile and Semivolatile Organic Compounds by GC-TMS in Support of Decision Quality Data

June 01, 2012

Environmental

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As analytical chemist(s), the data collected from samples we test represent information. That information may be required to direct environmental clean-up operations, help insure worker safety, or guide decisions for an emergency response to a chemical incident.

Radio Ion Chromatography

June 01, 2012

Pharmaceutical/Drug Discovery

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Positron emission tomography (PET) is one of the most powerful noninvasive diagnostic tools for tracing organ functioning. Quality control of the short-lived radiopharmaceuticals is challenging, not at least because of the tough time limits, the radiation issue, and the near nanomole radiotracer quantities.

Purge-and-Trap GC Analysis of Methane in Water Samples Associated with Hydraulic Fracturing

June 01, 2012

Environmental

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Shale gas reservoirs, such as the Marcellus shale reserve in Pennsylvania and Barnett shale reserve in Texas are a growing source of natural gas in the United States. Hydraulic fracturing or "fracking" involves pumping water, sand, and chemicals at extremely high pressure into deep underground wells to crack open hydrocarbon-rich shale formations and extract natural gas.

Vol 30 No 6 LCGC North America June 2012 Application Notebook PDF

June 01, 2012

Issue PDF

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Click the title above to open the LCGC North America June 2012 Application Notebook, Vol 30 No s6, in an interactive PDF format.