Author



S.-S. Cai

Latest:

Atmospheric Pressure Photoionization — The Second Source for LC-MS?

This article explores the progress that atmospheric pressure photoionization (APPI) has made in its relatively short history for LC–MS analysis. Specifically, the authors examine the combination of APPI and electrospray ionization (ESI).


Yvan Vander Heyden

Latest:

Advances in Supercritical Fluid Chromatography for the Analysis of Chiral and Achiral Pharmaceuticals

This article provides an overview of the most recent advances in the field of chiral and achiral separations in SFC. This involves research focused on the most critical parameters in SFC separations, but also on practical issues such as the serial coupling of columns.


Sandeep Patil

Latest:

Synthesis and Structural Elucidation of Impurities in Ramipril Tablets

Ramipril impurities D and E are well-known degradation products of ramipril in the finished dosage form. A significant amount of an additional impurity was detected in ramipril tablets by an isocratic reversed-phase high performance liquid chromatography (HPLC) method on a short column. The structure of this impurity was proposed based on liquid chromatography–mass spectrometry (LC–MS) data using an electron spray ionization source. Structural elucidation using nuclear magnetic resonance (NMR) and infrared (IR) spectroscopy was facilitated by a newly developed preparative isolation method. This impurity was characterized as (2R,3aR,6aR)-1-[(R)-2-[[(R)-1-(ethoxycarbonyl)-3-phenylpropyl]amino]propanoyl]octahydrocyclopenta[b]pyrrole-2-carboxylic acid (impurity L). Its identification, synthesis and characterization are discussed.


Achim Sprauer

Latest:

Characterization of PEGylated Lysozyme by Size Exclusion and Ion Exchange Chromatography

PEGylation, the process by which polyethylene glycol (PEG) chains are attached to protein and peptide drugs is a common practice in the development of biopharmaceuticals to prolong serum half-life and improve pharmacokinetics of a drug. There is increasing demand for chromatographic methods to separate the modified isoforms from the native protein. This application note describes the use of size exclusion and ion exchange chromatography for the characterization of PEGylated lysozyme.


Thomas Arthen-Engeland

Latest:

New Generation of GC/High Resolution TOF-MS: APCI/APLI Source for Increased Flexibility

A new APCI/APLI source enables a high resolution TOF-MS to be coupled on LC and GC, thus increasing flexibility and performance of TOF-MS in combination with GC.


Kurt Hostettmann

Latest:

Modern Countercurrent Chromatography

CCC is an excellent alternative to avoid the problems associated with solid-phase adsorbents, which include irreversible adsorption of sample and the need to replace expensive columns. As a result, CCC is gaining popularity as a purification tool.


Jeremy Dowling

Latest:

Performance Qualification of HPLC Instrumentation in Regulated Laboratories

With the forthcoming USP monograph <1058>, many laboratories are in the process of reexamining their high performance liquid chromatography (HPLC) instrumentation qualification practices. This article demystifies the qualification procedures and proposes a well designed, easy and simple set of experiments upon which to establish internal standard operating procedures (SOPs) for the complete qualification of HPLC instruments. A key concept is the development of a consistent test system, comprised of premade test solutions, a prequalified HPLC column, standardized protocols, and validated software that can be prepared in-house or purchased commercially as a kit. This system can be applied to any HPLC system worldwide, to produce comparable test results under uniform conditions. The test system is designed to be rapid, with a comprehensive performance qualification being completed in about 2 h for isocratic, and 3 h for quaternary gradient systems.


N.P. Shetgiri

Latest:

Synthesis and Structural Elucidation of Impurities in Ramipril Tablets

Ramipril impurities D and E are well-known degradation products of ramipril in the finished dosage form. A significant amount of an additional impurity was detected in ramipril tablets by an isocratic reversed-phase high performance liquid chromatography (HPLC) method on a short column. The structure of this impurity was proposed based on liquid chromatography–mass spectrometry (LC–MS) data using an electron spray ionization source. Structural elucidation using nuclear magnetic resonance (NMR) and infrared (IR) spectroscopy was facilitated by a newly developed preparative isolation method. This impurity was characterized as (2R,3aR,6aR)-1-[(R)-2-[[(R)-1-(ethoxycarbonyl)-3-phenylpropyl]amino]propanoyl]octahydrocyclopenta[b]pyrrole-2-carboxylic acid (impurity L). Its identification, synthesis and characterization are discussed.



Froseen Dahdouh

Latest:

Chemometrical Experimental Design-Based Optimization Studies in Capillary Electrophoresis Applications

A synopsis of our work detailing the use of chemometric response surface methodology (RSM) in two capillary electrophoresis (CE) studies is described.



Vita Knudson

Latest:

Additional Studies in the Separation of PEGylated Proteins by Reversed Phase Chromatography

Additional studies were undertaken to better understand the chromatographic behavior of PEGylated proteins in an effort to improve purification and characterization techniques of such proteins. Proteins were PEGylated using larger (20 KDa and 40 KDa) PEGylation reagents that are commonly used in pharmaceutical drug development. Generated PEGylated proteins were separated from unmodified proteins using different reversed phase medias (Jupiter® C4 and Jupiter® C18). In these studies it was found that the Jupiter C18 media provided the best separation of PEGylated proteins from their unmodified counterparts. Such results further clarify good method starting points for developing analytical and preparative separations of PEGylated proteins.


Michael Zumwalt

Latest:

The Use of Accurate Mass and MS-MS for the Analysis of PPCPs in Water

The United States Geological Survey (USGS) has found pharmaceuticals and personal-care products (PPCPs) containing known or suspected endocrine-disruptors in U.S. rivers. As such, it is important to use adequate techniques to help identify these compounds and possible metabolites.


Sudesh Bhure

Latest:

Synthesis and Structural Elucidation of Impurities in Ramipril Tablets

Ramipril impurities D and E are well-known degradation products of ramipril in the finished dosage form. A significant amount of an additional impurity was detected in ramipril tablets by an isocratic reversed-phase high performance liquid chromatography (HPLC) method on a short column. The structure of this impurity was proposed based on liquid chromatography–mass spectrometry (LC–MS) data using an electron spray ionization source. Structural elucidation using nuclear magnetic resonance (NMR) and infrared (IR) spectroscopy was facilitated by a newly developed preparative isolation method. This impurity was characterized as (2R,3aR,6aR)-1-[(R)-2-[[(R)-1-(ethoxycarbonyl)-3-phenylpropyl]amino]propanoyl]octahydrocyclopenta[b]pyrrole-2-carboxylic acid (impurity L). Its identification, synthesis and characterization are discussed.


Huilan Chen

Latest:

LC–MS-MS Determination of Malachite Green and Leucomalachite Green in Fish Products

Although not currently used in U.S. or European aquaculture, malachite green (MG) is still an effective and inexpensive fungicide that is used in other countries, particularly in Asia. During metabolism, MG reduces to leucomalachite green (LMG) (Figure 1), which has been shown to accumulate in fatty fish tissues. Trace levels of MG and LMG residues continue to be found in fish products. In a 2005 report, MG was found in 18 out of 27 live eel or eel products imported from China to Hong Kong local market and food outlets, resulting in a government recall and destruction of all remaining products (1).


Makoto Hashimoto

Latest:

Investigation of Transferrin Structure via Novel Electron Capture Dissociation Techniques Using a Hybrid Linear Ion Trap Time-of-Flight Mass Spectrometer

Protein and peptide analysis via tandem mass spectrometry (MS-MS) has resulted in a wealth of information regarding protein identification, structure, and abundance levels over the past 10 years. Techniques such as neutral loss scanning and collision-induced dissociation (CID) have been especially helpful in facilitating the identification of a multitude of previously unknown sites of protein phosphorylation. However, many of the techniques used to obtain this information are labor intensive and work inconsistently. To address this problem, much effort has been put forth to find alternative methods of fragmenting peptides and proteins that are less difficult and applicable to a wide gamut of peptide classes. Examples of recently developed dissociation techniques include infrared multiphoton dissociation (IRMPD) and electron transfer dissociation (ETD). The implementation of these new techniques has widened the spectrum of peptides amenable to tandem mass spectral analysis.


Deborah Hartley

Latest:

Charged Aerosol Detection in Pharmaceutical Analysis: An Overview

Over the past several years, charged aerosol detection (CAD) has become a widely used technology in the pharmaceutical laboratory. From formulation to stability and even quality control, many analysts are turning to this technology due to its advantages of sensitivity, ease of use, dynamic range, and applicability to a wide range of analyses in the drug development process. In this article, we will examine the operation and use of CAD in a regulated environment, briefly address method development and validation specifics, and highlight a few examples illustrating some of its advantages when used in the pharmaceutical laboratory.


Michelle L. Owens

Latest:

Separation, Identification, and Quantitation of Water-Soluble Vitamins by HPLC

The authors set out to perform a separation of seven water-soluble vitamins without the use of ion-pair reagents.


Christian Neusuess

Latest:

Multitargeting Pesticides

The usefulness of liquid chromatography–mass spectrometry–mass spectrometry (LC–MS-MS) methods for the unambiguous identification and quantification of pesticides in complex matrix samples is well known. Triple-quadrupole systems have proven to be useful for this task because of their high specificity in MS-MS mode and their low detection limits. However, working in MS-MS mode makes any MS system blind to other compounds of interest.


Lin Lu

Latest:

Fast Multi-Residue Pesticide Analysis Using Triple Quadrupole GC–MS-MS

H-SRM provides excellent selectivity for accurate identification and quantification of pesticides in matrix, demonstrating high productivity for effective control at international maximum residue levels (MRLs).


Stone D.-H. Shi

Latest:

Characterization of a Complex Protein Mixture Using nanoLC-LIT-TOF Mass Spectrometry

The nanoLC LIT-TOF approach combines multiple capabilities that improve the ability to characterize complex protein mixtures significantly.


Joseph L. Oliphant

Latest:

CUSTODION ™ SPME Syringe for Rapid Sample Collection and Sample Preparation of Drinking Water for the GC–MS Determination of Trihalomethanes

The CUSTODION™ SPME Syringes are a series of novel solid phase micro extraction syringes that incorporate Supelco Analytical's® (Bellefonte, Pennsylvania) SPME fiber technology. The SPME syringes are fabricated with injection-molded components and the device resembles a ball-point pen. The Supelco Analytical® SPME fiber assembly is housed inside the syringe.


Mark Collins

Latest:

Performance Gains Using Hydrogen Carrier Gas in Refinery Gas Analysis

Escalating costs and increasing demands for helium, coupled with diminishing helium supply, have given rise to the investigation and use of hydrogen as an alternate choice of carrier gas for use in gas chromatography (GC) applications. This application note illustrates that the use of hydrogen as a carrier gas as an alternative to helium in refinery gas applications is not only possible, but also results in improved performance and higher sample throughput.


Krishna M. Kallury

Latest:

A Simplified Approach to Optimize SPE Method Development with Downstream LC–MS Analysis Allowing 100% Organic, Basified Injection Solvents

Automated solid-phase extraction (SPE) has been used extensively with liquid chromatography–tandem mass spectrometry (LC–MS-MS) to facilitate high-throughput analysis in the pharmaceutical, diagnostic, and forensic toxicology areas. In this work, we demonstrate the use of a systemized approach to SPE method development and LC–MS-MS analysis. This approach provides dramatic savings in analysis time and takes advantage of new innovations in high performance liquid chromatography (HPLC) columns to provide the cleanest extracts for LC–MS injection.


Roselle Visaya

Latest:

Characterization of a Complex Protein Mixture Using nanoLC-LIT-TOF Mass Spectrometry

The nanoLC LIT-TOF approach combines multiple capabilities that improve the ability to characterize complex protein mixtures significantly.


Ian Acworth

Latest:

An Easy Way to a Fast Universal Method for Surfactant Analysis

Surfactants present a real challenge to the analytical chemist as they are a very complex class of chemical compounds.


Neal M. Fox

Latest:

Stability of Formic Acid in Methanol Solutions and the Implications for Use in LC–MS Gradient Elution Analysis

Dilute formic acid solutions in methanol were found to decline in acid content with time, the extent of the decline depending upon the initial amount of water present in these solutions. The effect of the formic acid concentration change upon the separation of peptides using high performance liquid chromatography (HPLC) is examined briefly.


Nobou Ochiai

Latest:

Gas Chromatography with Soft Ionization Mass Spectrometry for the Characterization of Natural Products

Soft ionization MS using GC–APCI-MS and GC–SMB-MS offers complementary identification power for the characterization of natural products, as illustrated by the identification of alkanes, sterols, long chain alcohols, and derivatized polar compounds in tobacco leaf extracts described here.


Werner Conze

Latest:

Characterization of PEGylated Lysozyme by Size Exclusion and Ion Exchange Chromatography

PEGylation, the process by which polyethylene glycol (PEG) chains are attached to protein and peptide drugs is a common practice in the development of biopharmaceuticals to prolong serum half-life and improve pharmacokinetics of a drug. There is increasing demand for chromatographic methods to separate the modified isoforms from the native protein. This application note describes the use of size exclusion and ion exchange chromatography for the characterization of PEGylated lysozyme.