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The End for High-Pressure Gas Cylinders?
High-pressure gas cylinders are a common sight in many laboratories: a default for supplying analytical instruments with their gas requirements, high-pressure gas cylinders are familiar and provide the gas that’s required, so it could be said that the old adage, ‘if it isn’t broke, don’t fix it’, could well apply. Despite this, increasing numbers of analytical instrument users are choosing to supply their GC FID, LC/MS and other types of instrument with gas via an analytical gas generator. Dr...
Fast Atom Bombardment (FAB) Technology Celebrates 30th Anniversary in Cardiff
Following the 2010 3-Day BMSS meeting in Cardiff, the same venue was chosen again to host the 2011 event. As a non-university venue there were misgivings about initially making such a move for the societies major event but overall, based on the largely positive feed back from delegates that attended in 2010, the move was judged a success and hence 250 delegates (50 less than in 2010 – a sign of the times rather than the meeting content surely?) made the journey to South Wales to update themselve...
High-Field Asymmetric Waveform Ion Mobility Separation and its Application to Small Molecule Analysis
High field asymmetric-waveform ion mobility spectrometry (FAIMS), also commonly referred to as differential mobility spectrometry (DMS), is an atmospheric pressure gas phase separation technique which exploits the difference between the mobility of an ion under high and low electric field conditions, as they pass between two electrodes. FAIMS can either be employed as a standalone mobility device or used as an orthogonal pre-separation technique hyphenated with chromatography and/or mass spectro...
Automation of a Complex, Multi-Step Sample Preparation Using the Standalone Agilent 7696A WorkBench
In analytical chemistry, sample preparation can be as simple as adding a solvent or as complex as performing chemical reactions to improve the instrumental measurements that follow. While sample preparation is a critical component to any chemical measurement, chemists rarely look forward to performing this job, especially if it is complex, boring and involves handling unpleasant chemicals. As a result, manual sample preparation can be the source of many errors and poor precision. To help reduce...
Overcoming the challenges of direct organic elemental analysis with ICP-MS
Analysing organic matrices for trace elements is a challenging proposition and frequently involves complex sample preparation steps. This is time consuming and potentially risks introducing contaminants or losing elements of interest. Sample digestion or wet ashing methods result in an aqueous matrix which can then be analysed by conventional ICP-OES or, where superior detection limits are required, by ICP-MS. However, the direct analysis of organic matrices by ICP techniques has historically pr...
Coupling Quadrupole ICP-MS with a Dual Syringe Pump Sample Introduction System for Fast and Accurate Determination of Trace Metals in Organic Solvents
The presence of trace metals in volatile organic solvents, even at trace level concentrations, has been associated with poisoning of industrial catalysts and subsequent contamination of final products. As a consequence, it is necessary that volatile organic solvents are analysed for trace metals in an accurate and reliable manner. Inductively coupled plasma mass spectrometry (ICP-MS) has been traditionally used to perform such analyses, however, the efficiency of the method is limited. This arti...
Report on 6th International meeting on MS and related techniques in advanced analytical science.
The "6th International MS Symposium" held in Manchester, UK 12-14th April was the latest in an occasional series of scientific meetings initiated (by Micromass) in 1998. Sponsorship of the meetings has now been taken over by Waters MS Technologies. The format is that of a legitimate scientific meeting, open to all, that typically attracts Ca 150+ delegates. The forward to the 1998 book of abstracts sums up the original vision, which remains true today - ‘a unique scientific forum focusing on hi...
HILIC After the Hype: A Separation Technology Here to Stay
Today Hydrophilic Interaction Liquid Chromatography (HILIC) is by far the fastest growing HPLC separation mode, currently being used by almost 20% of the HPLC instrument owners [1], although the relative number of applications still is considerably fewer. Does this mean HILIC is yet another technology-hype on the separation science scene, and that the interest will soon vanish? We believe not. This paper reviews the reasons behind the remarkable rise of HILIC and based on that, tries to predict...
From Atoms to Biomolecules: Celebrating the technological innovations in mass spectrometry on the 30th anniversary of the development of Fast Atom Bombardment (FAB)
British Mass Spectrometry Society - Annual 3-day Meeting at Cardiff City Hall, 11th - 14th September 2011 After the tremendous success last year of their first conference out of an academic setting, the BMSS are returning to Cardiff City Hall in September 2011. The purpose of this conference is, in line with BMSS aims, to provide an educational forum to discuss issues and applications associated with the use of mass spectrometers.The conference is designed to include and encourage an open exc...
The Technical and Clinical Benefits from Measuring 25 OH Vitamin D by LC- MS/MS
A dramatic explosion of interest in the clinical effects of Vitamin D and its metabolites in the past 5-10 years has stimulated a massive increase in requests for the measurement of 25 Hydroxy Vitamin D (25 OH D) in Clinical Chemistry laboratories throughout the world. Vitamin D can play an important role not only in the classical and well described area of bone health, where the re-emergence of rickets in population subgroups within the UK is a worrying problem and the role of 25 OH D in preven...
Oligonucleotide Biopolymers – Future Challenges for Chromatography
Synthetic Oligonucleotides as Therapeutic Medicines Synthetic oligonucleotides are an exciting new class of biomolecules capable of treating many disorders, which are currently not amenable to existing drugs, including viral infections [1], respiratory disorders [2], cancers [3] and rare diseases [4]. Current interest has been largely fuelled by two key events: firstly, Fire and Mello’s Nobel-prize winning discovery of gene silencing by RNA interference (which helped to improve our understandin...
The Identification of Illegal Anabolic Steroids in Customs Seizures by GCMS and High Resolution LCMS
There have been numerous reports in the news over the last few years of new drugs of abuse becoming available on the UK market. These have included mephedrone, benzylpiperazine and the so-called synthetic cannabinoids found in ‘Spice’ type herbal high products. These have all led to revisions of the misuse of drugs act in an attempt to control their distribution and use. A slightly older problem is the importation of anabolic steroids. In the year 2008/9 there were 802 seizures of anabolic stero...
Recent Developments in Type C Stationary Phases: Exploiting the Versatility of Silica Hydride Materials
TYPE C™ silica is a relatively new chromatographic material that has been finding ever-increasing use in the last few years. The properties exhibited by these stationary phases are often significantly different than the ordinary silica used for most commercial products. While all TYPE C phases can be utilised in the reversed-phase, organic normal phase and aqueous normal phase modes, there are some unique capabilities within each retention mode that have resulted in innovative method development...
The Identification of Illegal Anabolic Steroids in Customs Seizures by GCMS and High Resolution LCMS - Simon Hudson
There have been numerous reports in the news over the last few years of new drugs of abuse becoming available on the UK market. These have included mephedrone, benzylpiperazine and the so-called synthetic cannabinoids found in ‘Spice’ type herbal high products. These have all led to revisions of the misuse of drugs act in an attempt to control their distribution and use. A slightly older problem is the importation of anabolic steroids. In the year 2008/9 there were 802 seizures of anabolic stero...
Recent Developments in Type C Stationary Phases: Exploiting the Versatility of Silica Hydride Materials - Joseph J. Pesek & Maria Matyska
TYPE C™ silica is a relatively new chromatographic material that has been finding ever-increasing use in the last few years. The properties exhibited by these stationary phases are often significantly different than the ordinary silica used for most commercial products. While all TYPE C phases can be utilised in the reversed-phase, organic normal phase and aqueous normal phase modes, there are some unique capabilities within each retention mode that have resulted in innovative method development...
Advances in Separation Science - The Chromatographic Spring Symposium & Annual General Meeting - Paul Ferguson
The Chromatographic Society’s Spring Symposium and Annual General Meeting will be held at the Novartis site in Horsham (West Sussex) on Wednesday 11th and Thursday 12th May 2011. The theme for the meeting is ‘Advances in Separation Science’ with a particular focus on pharmaceutical drug discovery. The Spring Symposium will be held over one-and-a-half days allowing for an extensive range of presentations from academics, industrial speakers and vendors, as well as significant exhibition and networ...
High Throughput and Rapid Response Gas Chromatography Mr Phillip James & Dr Mark Landon
Have Large Cumbersome Air Blown Gas Chromatography Ovens Had Their Day? Since the late 50’s, conventional gas chromatographs (GC) have been designed in much the same way, with a heated circulating air oven for the column and block heater ovens for the injector and detector. Evolutionary development of the column oven has been influenced by the improvement in column technology from the original large diameter packed columns to todays small bore wall coated capillary columns with their impressive...
Vacuum Ultraviolet Spectroscopy - Rob Morris
A variety of materials have spectral signatures in the vacuum ultraviolet (VUV) region of 10–200 nm. VUV spectroscopy is useful for biomedicine, semiconductor testing and other applications. Because the spectral response of standard silicon charge-coupled device (CCD) detectors drops off rapidly at wavelengths as long as 400 nm, and because oxygen and water absorb in the VUV spectral band, maintaining sufficient signal outside a vacuum is not possible. Nitrogen purging of the spectrometer helps...
Near-Infrared Spectroscopy - Rob Morris
Near-infrared spectroscopy is a common analytical technique for chemistry and process control, where typical applications include identification of species and determination of water and fat content. New detector and optical bench options make it possible to configure miniature fibre optic near-infrared spectrometer setups for high-resolution applications such as laser and optical fibre characterisation. Laser Analysis using NIR spectroscopy Characterisation of laser lines – examples include s...
Sensitive Femtogram Determination of Aflatoxins B1, B2, G1 and G2 in Food Matrices using Triple Quadrupole LC/MS - Yang Chen and Jack Cappozzo
A simple and inexpensive sample cleanup procedure based on a dispersive solid phase adsorption approach (C18) is effective in removing background matrix contaminants for reliable determination of aflatoxins in food at the femtogram level by triple quadrupole LC/MS. This application demonstrates fast analysis time (< 6 min) with good chromatographic resolution and separation for all four aflatoxins. Standard curves for each aflatoxin analyte show good linearity (> 0.998) across a wide concentrati...
British Mass Spectrometry Society – Should you be a part? - Dr Susan Crosland
The British Mass Spectrometry Society has been representing the UK mass spectrometry (MS) community for over 40 years, and has many oversees members too. Its aim has always been to promote the education of scientists in MS - from the early days when it was just starting as an accessible technique, to today when the range of applications in which it is used is expanding dramatically. The Mass Spectroscopy Group (MSG) was set up in the UK in 1965, and its first meeting was that year at University...
Is there any such thing as a free hormone? Opportunities for online TFC-LC-MS/MS analysis of serum free steroids - Michael Wright, Lewis Couchman & David J Halsall
The majority of steroid and other small molecule hormones are extensively bound to carrier proteins in the blood stream. Whilst there is debate regarding the function of these carrier proteins there is a considerable body of evidence to suggest that the concentration of unbound or ‘free’ hormone is the most biologically and clinically relevant measure of hormone activity. This is commonly cited as the ‘free hormone hypothesis’ [1], the underlying assumptions being that: i) the hormone receptor i...
Chromatography…but not as we know it.- GlaxoSmithKline, Pfizer UK Group Ltd, Dynamic Extractions Ltd & Brunel Institute for Bioengineering
The use of countercurrent chromatography (CCC) as a preparative technique is seen to occupy a niche area of separation science and is largely used to isolate natural products. However, the technique has considerable untapped potential both at the laboratory preparative scale and also at larger scale. Introduction This article gives a chromatographer’s perspective of the potential of countercurrent chromatography (CCC) in the pharmaceutical industry, specifically relating to highperformance cou...
Using GC-MS/MS for Superior Sensitivity, Specificity and Precision in Free Testosterone Analysis - Rohan A. Thakur, Clark Williard and Agnita Rajasekaran
This article discusses biologically important steroid measurements which have, in the past, seen a lack of analytical sensitivity. Examples include determination of testosterone levels in women and children and oestrogen levels in post-menopausal women. The article gives insight into the analysis of free testosterone at physiologically relevant levels in plasma ultra-filtrate, concentrating on the sensitivity, specificity, precision and accuracy advantages offered by GC-MS/MS. INTRODUCTION Un...
Mass Spectrometry for a Changing World - Bernie Monaghan
As the Universities of Cardiff and Swansea have long held a renowned position in the world of Mass Spectroscopy via their output of well known academics and post graduate students, it seemed appropriate that the nomadic 31st BMSS 3 day meeting should find its way to the Cardiff City Hall (September 5-8th). Dr John Langley, the outgoing Chairman of the BMSS, noted in his letter to delegates that the fact that this constituted a quantum shift away from the usual academic campus environments which...
Analysis of Samples from the Gulf of Mexico Oil Spill by GCxGC-TOFMS - Leco Corporation
Two petroleum samples from the Gulf of Mexico Oil Spill were obtained: a Well Head Source Oil sample and a sample of Red Mousse. The Well Head Source Oil sample was collected by a Remotely Operated Vehicle (ROV) at the initial leaks in the damaged riser pipe. The Red Mousse sample was collected on the surface in the offshore marine environment. It had not been exposed to the surf zone. The samples provided had already been diluted in dichloromethane and had internal standards added prior to shi...
HPLC Assay of Water-Soluble Vitamins, Fat-Soluble Vitamins, and a Preservative in Dry Syrup Multivitamin Formulation - Suparerk Tukkeeree and Jeffrey Rohrer
INTRODUCTION Vitamins are vital to human development and long-term health; therefore, infants are usually prescribed a vitamin supplement to ensure they receive the recommended daily allowance of each vitamin. Children under one year of age are usually given this supplement in liquid form. This supplement can be produced as a dry syrup using a powdered preparation to which the pharmacist adds liquid to produce the dosage form for the patient. The work shown here describes an HPLC method to qua...
Agilent 6490 Triple Quadrupole LC/MS System with iFunnel Technology Ultra Sensitive Quantitative Performance - Agilent Technologies
Unmatched quantitative performance for the most challenging analyses The Agilent 6490 Triple Quadrupole LC/MS System incorporates iFunnel technology to give new levels of sensitivity for the most challenging quantitative analyses in pharmaceutical, clinical, food safety, and environmental applications. The quantitative power of the 6490 Triple Quadrupole is enhanced by an extended linear dynamic range. The 6490 Triple Quadrupole LC/MS delivers: • 10 X increase in sensitivity • Up to six orde...
Fluorine Detection in Drinking Water Using HR-CS AAS - Heike Gleisner
Due to its high electro negativity the element fluorine is the most reactive non-metal and thus does not occur in elementary, but only in combined form. Fluorine is the most widespread halogen. Its share in the earth’s crust is approx. 0.08%. It occurs in large quantities in apatite Ca5(PO4)3(OH,F) and in fluorite CaF2 as well as in the almost exhausted cryolite Na3AlF6 [1]. It is therefore no surprise that fluoride is also found in almost all water bodies - although the fluoride concentration...
UHPLC – A Small Step for Man, or a Giant Leap for Mankind? - Stuart Jones
In the mid 1990’s, HPLC was being described as a mature product. Most of the development was considered to have been done, and soon it would become a catalogue product like a hotplate stirrer. How far from reality that has turned out to be. HPLC is developing faster now than at any time since it was first introduced. Just think of the changes with mass spec, nano HPLC, high temperature HPLC, column developments, and by no means least, UHPLC. At its outset in the early 1970’s, HPLC used column...
A Case of Pesticide Poisoning: The Use of a Broad-Scope Tof Screening Approach in Wildlife Protection
INTRODUCTION As fragile ecosystems struggle to survive the impact of human domination of the environment, wildlife protection becomes increasingly important. While it is always preferable to safeguard living specimens in their native habitats, sadly, it is sometimes necessary to deal with the consequences of human interaction with vulnerable animals. Here we describe the use of a ToF screening approach in an incident of pesticide poisoning of a protected bird of prey. The red kite (family: acc...
Glycan Analysis Opens Up New Possibilities For Mass Spectrometry
Once again the mighty ASMS Conference flexes its muscles and heads into town, on this occasion Salt Lake City, to allow practitioners of the technique to meet, network, hear presentations from the great and the good, view poster sessions and see the latest offerings from the manufacturers and suppliers. The scale and credibility of this scientific meeting is certainly having an effect on the attendance on more generalist scientific meetings in North America such as the Pittsburgh Conference on...
High Throughput Screening for Phthalates in Toys and Childcare Articles Using the Agilent 6140 Single Quadrupole LC/MS System and Analytical Studio Browser Software
The European Commission has prohibited commercialisation of toys or child care articles containing more than 0.1% by weight of any of the following six phthalates: di-isononyl phthalate (DINP), di(2-ethylhexyl) phthalate (DEHP), di-n-octyl phthalate (DNOP), di-isodecyl phthalate (DIDP), butyl benzyl phthalate (BBP) and dibutyl phthalate (DBP). In addition, various other regulatory agencies throughout the world have banned the excessive use of these phthalates in toys[1]. In this Application No...
Oligonucleotides: The Next Big Challenge for Analytical Science
It is now over forty years since I started my career in analytical chemistry and during that time I have been privileged to witness many significant advances in the science and technology that underpin this important branch of chemistry. Most of these advances have arisen as a result of challenges from trace level analyte determinations, complex matrices, subtle structural idiosyncrasies and the omnipotent demand to make everything run faster and more reliably. One of the most challenging analys...
Prominent Speakers Captivate Audience
At Science World – The Fisher Scientific Laboratory Experience visitors were treated to two thought provoking seminars from Lord Professor Robert Winston and Professor David Bellamy. Speaking to a packed auditorium, Professor Winston questioned how scientists engage with the general public, particularly in relation to ethical issues. “It is very clear in a modern society, (that) we have to be much more responsive and recognise that the adverse effects of the things that we do does impact on soc...
Recent Advances in the Methodology for Environmental and Food Matrix Analysis - a report on the 5th National Conference on Environmental Mass Spectrometry
This meeting, held on March 24th at the University of Chester, was an environmental mass spectrometry special interest group (EMSSIG) series event forming a part of the BMSS SIG meetings. The main theme focussed on ‘Recent Advances in the Methodology for Environmental and Food Matrix Analysis’ and was linked to the Food and Nutrition SIG coordinated by Dr Simon Hird, thereby forming part of a conference week, during which three meetings were organised by Professor Chris Smith, which highlighted...
Liquid-Liquid Chromatography Instrumentation for Laboratory Preparative & Process Chemistry
Liquid-Liquid Chromatography (L-LC) Instrumentation, also referred to as Counter Current Chromatography (CCC, HSCCC, HPCCC), and Centrifugal Partition Chromatography (CPC), designs have existed for 60 years. Solid-Liquid Chromatography (S-LC) techniques include Open Tubular, Flash, MPLC and HPLC also have an extensive history. For the vast majority of applications both L-LC and S-LC have a stationary and a mobile phase. With S-LC the stationary phase is often a liquid, immobilised by bonding on...
LCMS: From Pharmacokinetics to Metabolomics
Bernie Monaghan (BM): Could you tell us a little about the unit and group in which you work at Sutton? Florence Raynaud (FR): I work at The Institute of Cancer Research (ICR) in the Section of Cancer Therapeutics. Our mission is to discover and develop new drugs to treat cancer. We have an impressive track record in drug discovery in oncology as four compounds (melphalan, chlorambucil, carboplatin and ralitrexed) originating from the ICR have gained regulatory approval. In addition, we have se...
Confirming Peak Identification in Bioanalytical Studies Utilising Xevo TQ MS Product Ion Confirmation
INTRODUCTION The accurate quantification of candidate pharmaceuticals in bioanalysis relies on the use of sensitive, specific methodology. The advent of atmospheric pressure ionisation sources, in the late 1980s, allowed the simple interfacing of liquid chromatography with tandem quadrupole mass spectrometry. The selectivity and sensitivity provided by LC/MS/MS has made it the technique of choice for bioanalytical studies. Bioanalytical scientists have relied on the specificity and sensitivity...
A Touch of Genius
In what has been a year of opportunity for visionary science led companies, it is comforting to report that innovation is alive and well, not only in the multi nationals, but, in some of the smaller scientific businesses also. Peak Scientific Instruments, the Scottish based, global gas generator manufacturer has enjoyed a buoyant year fuelled, behind the scenes, by a desire to improve its products and become a ‘best of breed’ manufacturer. To accelerate this period of product development and gr...
The Fascinating History of the Development of LC-MS; a Personal Perspective
Today LC-MS is considered as a commonplace analytical tool that has been around for years. Most users do not give a second thought to the history of the development of this fascinating technique. It is twenty years since the first commercial instrument dedicated to atmospheric pressure ionisation (API) was produced by a small and then unknown company called Sciex, and so now is probably a good time to review some of the significant challenges that were faced to develop the technique. I would...
LCMS: From Pharmacokinetics to Metabolomics
My team is involved in drug metabolism and pharmacokinetics of novel chemical entities and in the clinical pharmacokinetic evaluation of some of our agents, which have reached Phase I/II clinical trials at The Royal Marsden Hospital... Bernie Monaghan (BM): Could you tell us a little about the unit and group in which you work at Sutton? Florence Raynaud (FR): I work at The Institute of Cancer Research (ICR) in the Section of Cancer Therapeutics. Our mission is to discover and develop new dru...
Analysis of Loratadine and Related Substances Using the ACQUITY UPLC H-Class System
Develop a method that is approximately five times faster and produces data of equal or better quality than current HPLC methods by using the ACQUITY UPLC H-Class System. This system provides an ideal solution for laboratories running USP compendial HPLC methods or that are looking to migrate current methods to the efficiency and cost-effectiveness of UPLC. GOAL Successfully transfer the compendial HPLC method for the analysis of Loratadine, as written, to the ACQUITY UPLC® H-Class System and s...
A Path to Greater Productivity in HPLC
The options facing the chromatographer have multiplied dramatically over the past few years. UHPLC, short fast columns, micro-bore, etc are all possible directions in which to move from the conventional HPLC column. Factor in the need to scale up for semi preparative or preparative use and the options increase again. In order to make the most cost effective choice, the whole process should be considered to determine the requirements to move from the current position to the required goal. All the...
LC-NMR – Who in Their Right Mind Would Even Consider it?
Bernie Monaghan (BM): Could you tell us a little about the group in which you work in Sunderland? Nicolas Haroune (NH): Chemispec was established in 2000 when the University obtained a grant from the ERDF (European Research Development Fund) to purchase analytical equipment with the aim of helping small and medium enterprises in the North East of England. 2 NMR spectrometers (500 and 300MHz), 1 mass spectrometer (Apex II FT/MS) were purchased. More particularly, the 500MHz spectrometer was equi...
Applications of Liquid-Liquid Chromatography Instrumentation for Laboratory Preparative & Process Chemistry
Liquid-Liquid Chromatography instrumentation (L-LC), also referred to as Counter Current Chromatography (CCC), and Centrifugal Partition Chromatography (CPC), design has been instigated and, championed largely by Academics at University and Research Institutes in USA, Japan, Europe and China. To date instrumental L-LC has not been universally adopted by chromatographers in many commercial sectors. Discussed is a scientific treatise from a commercial viewpoint, of usage and design advantages and...
CHROMATOGRAPHERS ARE EuSSS Never heard of EuSSS? Read this Article and you will have...
Do you want to keep in touch with scientists who share the same or similar interests? Do you want to know what’s happening in your speciality across Europe rather than just within your own country? Do you wish to travel to scientific meetings and share your knowledge with others who will understand and appreciate it? The founders of EuSSS wanted all these things and have set up the means for achieving them and more. It is very simple to join and costs you nothing. Analytical chemists who prac...
How to Choose the Right Miniature Spectrometer
Choosing the right miniature spectrometer is very application-dependent, so there are a few questions that need to be asked. What are you trying to measure and why? How fast do you need measurements? Where is the sample and who will be operating the instrument? The design also involves money, so it is important to have a cost target for the system in mind as well. To configure a spectrometer, there are some important choices that need to be made, such as the choice of wavelength range, optical...
Fully Automated QuEChERS Clean up and LC/MS-QQQ Analysis of Pesticides in Fruits and Vegetables
This article outlines a fully automated method based upon the widely used QuEChERS (quick, easy, cheap, effective, rugged and safe) methodology -, for the extraction and clean up of pesticide residues in samples of fruit and vegetables. With the number these measurements set to rise in the near future, the commercial case for the automation of this time consuming, manual method is compelling. The QuEChERS method uses an acetonitrile extraction followed by the salting out of water from the sampl...
Using Mass Spectrometry to Provide Accurate Chemical and Bio-Measurements
As the UK’s designated National Measurement Institute (NMI) for chemical and bio-measurements, LGC has a major role to play in helping to improve the accuracy and reliability of chemical and bio-analytical measurements that are important to the UK’s industrial competitiveness and quality of life. LGC’s measurement science is recognised throughout the world and many of our experts represent UK metrology interests through European and international organisations. The UK National Measurement Syst...