HPLC and GC Articles

Electromembrane Extraction

This mini-review of a new sample preparation technique called "electromembrane extraction" demonstrates how the combination of an electroextraction with hollow-fibre liquid-phase microextraction can lead to a very selective, rapid sample preparation method for the extraction of charged substances from complex matrices such as plasma, breast milk and urine. Several important parameters for successful extraction are presented and application examples of various analyte-matrix combinations are tabulated.
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LCGC Europe, Mar 1, 2010

Chromatography Standards Certificates

Standards are as important in chromatography as columns, mobile phases, injectors and detectors.1 There's hardly an analytical laboratory to be found that does not stress the need for the certification of all components involved in an analysis. Quite remarkably though, standards are not always thought of as being an essential part of a certified analysis because many analysts prepare their own standards, while the other attributes are almost always purchased ready-made from a certified supplier.
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LCGC Europe, Mar 1, 2010

Spring Cleaning

Laboratory instrument systems require regular maintenance for consistent and reliable results. In this month's "GC Connections", John Hinshaw addresses the regular maintenance of gas chromatography components that can become compromised in the course of normal use, including symptoms, causes and remedies.
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LCGC Europe, Mar 1, 2010

Enhancing Signal-to-Noise

The signal-to-noise ratio (S/N) in a liquid chromatography (LC) separation is usually defined as shown in Figure 1. The noise is measured between two lines bracketing the baseline and the signal is measured from the middle of the baseline to the top of the peak. S/N is merely the signal divided by the noise. There are some other ways to determine S/N, but that is not the point of the current discussion. My comments here will apply no matter what technique you use for measurement and calculation of S/N.
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LCGC Europe, Mar 1, 2010

Direct-EI in LC–MS

Coupling liquid chromatography (LC) and mass spectrometry (MS) is always a 'work in progress' with the final goal of providing the most sophisticated detector capable of identifying and quantifying organic and inorganic compounds at trace level. Well-established LC-MS interfaces and several novel ones are constantly being developed and different operating strategies have been adopted to overcome the apparent difficulties of coupling the two techniques.
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LCGC Europe, Mar 1, 2010

Diamonds as a Stationary Phase

Our group started investigating diamond as a potential stationary phase for chromatography in 2005, following a discussion about the possibility of fractionating such abrasive microparticles based on size. I was surprised by the amount of different types of synthetic diamonds that have been manufactured by large-scale industrial production and their easy availability.
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LCGC Europe, Mar 1, 2010

Selection of Columns for GCxGC Analysis

Multidimensional separations are performed by combining single analytical separation columns in such a way to greatly enhance peak capacity for the separation of complex multi-component samples. Comprehensive multidimensional gas chromatography (GCxGC) employs largely independent first- and second-dimension separation mechanisms and typically generates peak capacity of the order of several thousand, making it a highly appropriate technology for the separation and analysis of complex multicomponent samples such as essential oils.
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LCGC Europe, Feb 1, 2010

Column Diameter, Linear Velocity and Efficiency

I recently had a question regarding some changes that took place in the 2009 edition of the US Pharmacopeia. In USP 32, General Chapter 621,1 the adjustments allowed to meet system suitability for liquid chromatography (LC) methods include a change in column internal diameter of +-25%. A change was made in USP 32 Supplement 2.2 This stated that column internal diameter "can be adjusted provided that the linear velocity is kept constant." The person was not sure how this adjustment of linear velocity should be made and wondered about what effect it would have on column efficiency.
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LCGC Europe, Feb 1, 2010

Analysis of Persistent Halogenated Organic Compounds

An important goal in the field of analytical chemistry is to achieve continual improvement in the analysis of persistent toxic pollutants. Halogenated organic compounds represent an important group of pollutants. They are used in a wide variety of applications such as flame retardants, fire suppressants, heat-transfer agents, surfactants and pesticides, mainly because of their chemical inertness and stability.
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LCGC Europe, Feb 1, 2010

A Global Approach to HPLC Column Selection Using Reversed Phase and HILIC Modes: What to Try When C18 Doesn't Work

Aqueous-organic mobile phases (for example, water-acetonitrile) have become preferred for high performance liquid chromatography (HPLC) analysis due to their wide availability, high quality, low toxicity, and compatibility with popular detection methods. Selecting the optimum column to work with aqueous mobile phases is an important part of HPLC method development. Given the vast number of choices and the lack of chemical detail about many column products, many analysts do not take time to explore column options in any systematic way.
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LCGC North America, Mar 1, 2010

The 2010 LCGC Pittcon Awards

Now in its third year, the LCGC Awards have quickly grown into one of the industry's premier honors for both emerging and veteran practitioners of chromatography. In this relatively short timeframe, the awards have built a prestigious list of awardees from all over the field and from a variety of different specialty areas, and this year in particular, generated a great deal of interest from all across the field of chromatography.
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LCGC North America, Mar 1, 2010

Spring Cleaning

Periodic maintenance is the mainstay of keeping laboratory instruments running at the peak of performance. Analysts can avoid many problems by proactive evaluation, repair, and replacement of critical system components on a regular basis. The alternative of allowing contamination to build up, syringes to wear out, or septa to leak only results in increased down-time compared to planned maintenance outages. Unplanned maintenance and repair is not predictable and in my experience, most such incidents occur at the worst time.
Journal: 
LCGC North America, Mar 1, 2010

Enhancing Signal-to-Noise

The signal-to-noise ratio (S/N) in a liquid chromatography (LC) separation usually is defined as shown in Figure 1. The noise is measured between two lines bracketing the baseline and the signal is measured from the middle of the baseline to the top of the peak. S/N is merely the signal divided by the noise. There are some other ways to determine S/N, but that is not the point of the current discussion. My comments here will apply no matter what technique you use for measurement and calculation of S/N.
Journal: 
LCGC North America, Mar 1, 2010

New Chromatography Columns and Accessories at Pittcon 2010: Part I

Pittcon 2010, referred to in its full name as the 61st Pittsburgh Conference on Analytical Chemistry and Applied Spectroscopy, returned to the massive Orange County Convention Center in Orlando, Florida, from February 28-March 5, 2010. This year's event hosted nearly 1000 instrument manufacturers and 1aboratory suppliers in more than 2000 booths. In addition to attending the exposition, the conferees listened to 2000 technical presentations, checked numerous company seminar rooms, or attended one of 140 short courses.
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LCGC North America, Mar 1, 2010

SPME with GC×GC and GC×GC–TOF-MS

Since the development of comprehensive two-dimensional gas chromatography (GCxGC) by Phillips and coworkers in 1990, and most notably in the past five years, GCxGC and multidimensional GC by heartcutting have become increasingly popular among analysts in a variety of disciplines (1). A number of recent reviews describe advances in GCxGC that demonstrate its high selectivity and ability to separate extremely complex mixtures, so these are not repeated here (2).
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LCGC North America, Feb 1, 2010

A History of Gas Chromatography

I was lucky to be around in the beginning of gas chromatography (GC). I heard about it in 1956, made my first injections in 1957, and am still working with it today. I was recently encouraged by LCGC's Editor-in-Chief David Walsh to write up some of the early history that I experienced, which I present here.
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LCGC North America, Feb 1, 2010

Column Diameter, Linear Velocity, and Column Efficiency

I recently had a question regarding some changes that took place in the 2009 edition of the United States Pharmacopoeia. In USP 32, General Chapter 621 (1), the adjustments allowed to meet system suitability for liquid chromatography (LC) methods include a change in column internal diameter of +-25%. A change was made in USP 32 Supplement 2 (2).
Journal: 
LCGC North America, Feb 1, 2010

Electromembrane Extraction

Recently, efforts have been devoted to the miniaturization of existing liquid-liquid extraction methods to make them more versatile and powerful. Reducing the use of hazardous organic solvents due to environmental and cost concerns, time reduction, ease of automation, possible online coupling, high-throughput capability, and the small amounts of matrix available are major incentives that have motivated scientists working towards miniaturization.
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LCGC North America, Feb 1, 2010

GC Method for Residual Solvents

Residual solvents in pharmaceuticals are organic volatile impurities left over from the synthesis of active pharmaceutical ingredients (APIs) or from the manufacturing processing of pharmaceutical products. Their levels are monitored and controlled for safety reasons (1-4) and for their potential impacts on the crystalline form, possibly affecting solubility, stability, and bioavailability (5). Analytical techniques were recently reviewed (6,7).
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LCGC North America, Jan 1, 2010

HPLC: Challenges to Food and Drug Safety

Bisphenol A (2,2'-bis[4-hydroxyphenyl]propane), or BPA, is a key industrial chemical used to make polycarbonate plastic and epoxy resins and is used to prevent food contamination in canned goods and other food packaging. BPA can be released from these materials and can induce adverse effects in humans including hormonal responses, because it mimics estrogen. BPA is consistently in the news as mothers worry about it leaching from their baby bottles and hikers from their water bottles.
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LCGC North America, Jan 1, 2010

Upgrading Gas Chromatography

Technologies for laboratory analysis advance continuously, just as do computer technologies or transportation technologies. Small advances tend to occur fairly often while major new technologies appear less frequently. As new capabilities become available, laboratories must decide whether to acquire them or to defer and continue to use what they already have.
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LCGC North America, Jan 1, 2010

Too Little or Too Much

The topics for this month's "LC Troubleshooting" column come from the attendees of some of the method-development and troubleshooting classes that I have taught recently. One of these problems involves a liquid chromatography (LC) method in which an occasional sample gives a peak that is too small. The second case is one in which the analyte peak appears when a drug-free placebo sample is run.
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LCGC North America, Jan 1, 2010

Seeing in the New Year... or Making Sure the Old One Leaves

By the time readers are opening the pages of this issue, we will all have turned the calendar on 2009 and left it behind for what will hopefully be a brighter 2010. Humorist Bill Vaughan once famously said of New Year's Eve: "An optimist stays up until midnight to see the new year in. A pessimist stays up to make sure the old year leaves." Given the financial year we all just experienced, my suspicion is there may be a few more people in the latter group than in the former this year. However, here at LCGC, we can't help but be optimistic about 2010.
Journal: 
LCGC North America, Jan 1, 2010

Upgrading Gas Chromatography

Technologies for laboratory analysis advance continuously, just as computer technologies or transportation technologies do. Small advances tend to occur fairly often while major new technologies appear less frequently. As new capabilities become available, laboratories must decide whether to acquire them or to defer and continue to use what they already have.

Journal: 
LCGC Europe, Jan 1, 2010