Application Notes: Pharmaceuticals

Robust hardware and automated software are critical to method ASTM D7169. The Shimadzu GC-2010, equipped with an advanced flow controller, has proven to be reproducible and effective, and Shimadzu distillation GC software has achieved automation by integrating calibration, integration, calculation, and report functions.

Porous ODS columns are the most popular reversed-phase columns used in today's laboratories.

LEAP has developed a new instrument for collecting the entire mobile phase stream during metabolic profiling HPLC–MS analyses into a sealed, 96-well, LTuma plate.

Gel permeation chromatography (GPC) is a very effective sample clean-up technique, key to an accurate and sensitive analysis of pesticide, PCBs, mycotoxin, PAHs, and other similar compounds.

The costs associated with pharmaceutical testing are considerable and many lab managers are seeking ways to reduce costs by reducing solvent usage and improving productivity while still using the LC instruments in their lab.

With many "blockbuster" drugs losing patent protection, there has been mounting pressure across the pharmaceutical industry to shorten the time to bring new chemical entities (NCEs) to market and reduce the overall cost. This requires concerted productivity improvement in many aspects of drug discovery and development by continuously adopting new enabling technologies.

Quantification of substances, such as drug impurities or library compounds when pure standards are not available is difficult yet often necessary.

Benzodiazepines are commonly assayed to determine therapeutic dose levels and for forensic investigation. These drugs are commonly prescribed to alleviate pain and therapeutic dosing needs to be monitored.

In pain management analysis, urine is often used as it is a copiously available bodily fluid that can be collected easily and used for analysis. Urine, however, can cause difficulties in analysis due to the variances in the endogenous nature of the urine matrix, which can impact the chromatographic separation and quantitation.

The U.S. EPA Office of Groundwater and Drinking Water released Method 524.3, "Measurement of Purgeable Organic Compounds in Water by Capillary Column Gas Chromatography/Mass Spectrometry, Version 1.0," in the Federal Register on August 3rd, 2009 (1, 2). This new method contains an updated list of 76 VOCs that includes fuel oxygenates and two emerging contaminants of interest.

Explosive compounds are widely used in warfare, mining industries, terrorist attacks, and civil constructions. Explosive contaminated soils are mostly found on firing points, impact areas, and training ranges. The explosive contaminates in soil are possible sources for surface and ground water contaminations, posing environmental and public health risks due to the compounds' toxicity, carcinogenicity, and mutagenicity.

Hamilton Company is best known for manufacturing precision fluid measuring products, including syringes for HPLC and GC. For the last 30 years Hamilton Company has manufactured HPLC resins and columns while developing separations for customers. Two of the separations are highlighted below.

Bisphenol A (BPA) is widely used in high production volume manufacturing of polycarbonate plastics (for example, food containers and plastic bottles) and epoxy resins (1).

Grapefruit juice was analyzed by gradient UHPLC for naringin - a flavanoid that gives it its bitter taste. A ZORBAX Rapid Resolution HD (RRHD) StableBond-C18 2.1 x 150 mm, 1.8 µm column resolved over 60 peaks including naringin in 7 min, and was re-equilibrated in just 3 min by operating at a high flow rate (0.8 mL/min).

The identification and quantification of drugs of abuse in blood (plasma, serum, whole blood) has become very common in the forensic medicine laboratory. Liquid-liquid extraction (LLE) has been traditionally used at a basic pH (pH = 9) for the extraction of amphetamines, cocaine and its metabolites, and opiates from blood.

Many methods have been proposed to determine acylglycerols in biodiesel samples. This analysis is commonly performed by GC/FID (ASTM D6584/EN14105 methods).

In the production of biopharmaceuticals, there may be different analytical requirements for groups performing clone section, formulations and stability, and quality control (QC).

The fully automated combustion ion chromatography (CIC) system presented here combines a highly efficient combustion system with the separation power of ion chromatography (IC).

This paper describes the use of the AB SCIEX TripleTOF 5600 LC–MS-MS system for the screening and identification of unexpected contaminants in lake water, demonstrating the value of high-resolution, accurate-mass data, and retrospective data processing for the identification of nontargeted compounds.

Methacholine chloride is a synthetic analogue of the neurotransmitter acetylcholine used to assess bronchial asthma of subjects in respiratory function labs and epidemiological field studies (1).

The speed and accuracy of software-assisted identification of metabolites can be further improved by combination with rule-based metabolite prediction software.

For many years, the use of guard columns has been advocated by column manufacturers and other experts to protect and extend column lifetime and performance of analytical columns from potential damage caused by the presence of chemical contaminants and microparticulates in the sample and mobile phase.

Heparin is well-known as an anticoagulant, antithrombotic drug. Chemically, it is a linear polysaccharide that is derived from animal tissues. For some time it has been known that heparin is not a homogeneous substance; rather, it is a heterogeneous mixture of molecules ranging in molar mass from less than 5,000 to more than 30,000 Daltons.

Since 2001 when they became available in North America, monolithic silica HPLC columns have become valuable analytical tools in the R&D and methods development laboratories.

The EcoSEC GPC System and a set of TSK-GEL mixed-bed columns, both available from Tosoh Bioscience, were used successfully for obtaining high quality MWD data of a series of block poly-β-alkylalanoids with HFIP as the mobile phase in under 15 min.

The RegisPack® chiral stationary phase allows for the enantiomeric separations of a wide variety of racemate classes.

The analysis of melamine in milk and other food products became urgent when first the pet food, and later the milk scandal were discovered in the U.S. and China.

One of the most important attributes of flexible fused silica capillary tubing is its outstanding strength. When made properly with a protective abrasion resistant coating and handled appropriately this material has proven to maintain its strength remarkably well.

Analyzing basic pharmaceuticals and peptides can be challenging with conventional ODS columns.

The U.S. EPA Office of Groundwater and Drinking Water released Method 524.3, "Measurement of Purgeable Organic Compounds in Water by Capillary Column Gas Chromatography/Mass Spectrometry, Version 1.0," in the Federal Register on August 3rd, 2009 (1, 2).