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In a recent review of blood alcohol casework performed by a forensics laboratory associated with a major metropolitan police force, I was again disheartened to find major deficiencies in method validation protocols. In this case, the analysts failed to check whether aqueous solutions for calibration and quality control were reliable surrogates for real blood samples.

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The determination of the chemical composition distribution of acrylic resins is not straightforward. Pyrolysis–gas chromatography (py-GC) analyses of acrylic resins can yield problems in the recovery of the hydroxyl and acid functional fragments that form. To overcome these problems pyrolysis–liquid chromatography (py-LC) can be performed. This article describes how the validation and quantification of hydroxyl acrylate-, hydroxyl methacrylate-, hydroxyl propylacrylate-, and hydroxyl propylmethacrylate resins by py-LC is performed. Furthermore, off-line size-exclusion chromatography (SEC) coupled to py-LC is performed to determine the chemical composition distribution over the molecular weight distribution of a core–shell waterborne acrylic resin.

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The 44th International Symposium of High Performance Liquid Phase Separations and Related Techniques (HPLC 2016), chaired by Professor Robert Kennedy, was held 19–24 June in San Francisco, California, USA, at the Marriott San Francisco Marquis. This instalment of “Column Watch” covers some of the highlights observed at the symposium, including stationary-phase developments, particle technology, and areas of growing application of high performance liquid chromatography (HPLC). In addition, trends and perspectives on future developments in HPLC noted from the conference are presented.

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One of the common threads in the six data integrity guidance documents published to date is the need to control any blank forms used in regulated GXP laboratories. This month’s “Questions of Quality” is focused on how to interpret the regulator’s requirements for this topic. We also pose the question: Is paper the best way to record regulated data?

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A universal generic high performance liquid chromatography (HPLC) or ultrahigh-pressure liquid chromatography (UHPLC) method with a primary modern column that works well for most drug analyses in a few minutes would be an attractive idea for many laboratories. With advances in column technologies, this ideal scenario is becoming more realistic, as demonstrated in the proposed 2-min generic method shown here. In addition, rationales for the selection of column and operating conditions are discussed, together with ways to extend this generic method as a starting point for stability-indicating applications by simple adjustments of gradient time and range.

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Ultrahigh-pressure liquid chromatography (UHPLC) instruments from different manufacturers and instruments with different configurations can produce significant variations in chromatographic separation. The variety in instrument configuration increases the complexity of the method development process, which now requires a more thorough evaluation of the effect of instrument variations on the method. The studies presented here determined the typical interinstrument variations in dwell volume, extracolumn dispersion, and mixing efficiency as measured by mobile-phase compositional accuracy. Additionally, the dwell volume and extracolumn dispersion were independently and systematically varied to evaluate the resulting impact on resolution for a small-molecule test mixture during gradient elution. To account for these interinstrument variations, dwell volume and wash-out volume method translation and adjustment techniques were evaluated.

While gas chromatographers may take their septa for granted, in fact these small and seemingly unremarkable polymer disks keep air out of the carrier-gas stream when used in an inlet and keep samples intact and uncontaminated when used in sample vials. Choosing the wrong septa can compromise method accuracy and repeatability as well as reduce column life in extreme cases. This instalment addresses septa for inlets and sample vials.

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The past couple instalments of “Sample Preparation Perspectives” have looked at current trends in the field. Another recent trend is dried blood spot analysis and other analysis methods using minute sample amounts. This month we take a quick look at the role of sample homogeneity and the determination of sample size. Microsampling approaches, including dried blood spots, are discussed.

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Significant benefits can be obtained by standardizing high performance liquid chromatography (HPLC) columns in a pharmaceutical development laboratory. Here is a story of how one organization attempted to encourage its staff to develop HPLC methods using fewer column brands and dimensions to reduce waste and efforts in method transfers downstream.

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A popular feature of The Chromatographic Society’s Golden Jubilee publication was an article by Waters describing their heritage and setting out their contributions to the development of chromatography. In this special feature, some of the companies who are regular exhibitors at Society events answer questions on the current and future status of chromatography.

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The first meeting in The Chromatographic Society’s diamond anniversary year brought together world‑renowned speakers alongside past presidents of the Society, delegates from academia and industry, and scientific instrument and technology companies at the Institute of Engineering and Technology in central London on 22 March 2016. The presentations included discussions on liquid chromatography (LC), supercritical fluid chromatography (SFC), and gas chromatography (GC) from both an academic and industrial perspective - providing excellent insight into the state-of-the-art in these techniques for the delegates.

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On the occasion of the Golden Jubilee of The Chromatographic Society, Peter Myers wrote “The Future of Chromatography” in The Chromatographic Society’s souvenir brochure. Now Peter revisits his chromatographic crystal ball to review his predictions and deliberate on what the future might now hold for separation scientists.

A theme for The Chromatographic Society Diamond Jubilee Year is to increase public awareness of chromatography. Often the general public, and even chromatographers themselves, fail to appreciate the importance of chromatography. Here Tony Edge, The Chromatographic Society Vice-President, discusses just how much chromatography underpins everyday life.

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Antibody related biopharmaceuticals represent one of the most dynamic segments of the pharmaceutical market. The analysis and monitoring of product titers in CHO cell cultures is one of the key tasks during development of new products. Cell line selection, optimization of expression rates, and process control need fast and efficient antibody quantification. Besides ELISA assays with known limitations with regard to reproducibility and precision, high performance liquid chromatography (HPLC) analysis using affinity chromatography is applied. This application note summarizes some performance data of a new Protein A affinity column for mAb titer analysis.

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This study describes a simple, quick approach for the sampling and analysis of nicotine, impurities, and flavour compounds in e-cigarette vapours. Combining thermal desorption (TD) with gas chromatography–mass spectrometry (GC–MS) analysis results in a versatile screening method for tackling the challenge of regulatory compliance and quality control in this rapidly expanding industry.

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Analyzing a broad range of semivolatile environmental pollutants at low levels requires a sensitive detector as well as an inert sample pathway. While semivolatiles analysis by methods such as EPA 8270 and EPA 625 typically does not require reporting sub nanogram-on-column concentrations, the latest generation of sensitive mass spectrometers and inert GC columns and inlet liners allow analysts to take advantage of the benefits of split injection while maintaining standard method reporting limits.

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Whole column imaging detection capillary isoelectric focusing (iCIEF) has been recognized as a powerful tool for biopharmaceutical development and quality control. Unlike conventional single point detection capillary electrophoresis (CE) systems, in which light absorbance or emission at a specific point along the separation capillary is monitored, iCIEF detects a line of light that is passed through and radiates from the entire separation capillary. As a result, sequential snapshots of the whole separation capillary at different times are obtained. This allows sample separation and interaction in real time to be observed during electrophoresis, enabling fast analytical method development, high resolution separation, and high sample throughput.