Application Notes: GC-MS

The CUSTODIONâ„¢ solid phase microextraction (SPME) syringe was used to rapidly sample and concentrate volatile organic compounds (VOCs) from water in 5 s. The VOCs were analyzed quickly and reliably in approximately 70 s using the GUARDIONâ„¢ -7 portable capillary gas chromatograph toroidal ion trap mass spectrometer (GC-TMS).

Melamine is an industrial chemical with a high nitrogen content that can cause kidney stones and lead to renal failure. In some instances, melamine has been added to baby formula and dairy products as a substitute for protein. This paper presents an efficient and definitive gas chromatography–mass spectrometry (GC–MS) method to identify melamine and related compounds based on the released US Food and Drug Administration (FDA) method.

This application details a fast, reliable and highly selective trace-level screening method for the quantification of polychlorinated biphenyls (PCBs) in environmental, food and biological samples, using gas chromatography and a triple stage quadrupole mass spectrometer. The analytical strategy is analogous to the well-established US Environmental Protection Agency (USEPA) Method 1668A.

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.

Screening for pesticide content is a common analysis that is done in laboratories where many samples need to be analyzed over a short period of time. The desire for a high-speed analysis is due to the need for a fast result from a potentially large volume of samples. A fast analysis is typically achieved through the use of high carrier gas flow rates in combination with temperature programming. A fast detector is needed in order to fully characterize the narrow chromatographic peaks generated from these experiments. TOFMS is ideal for detecting these narrow peaks because of its fast acquisition rate over a full mass range at all times during the experiment. In addition, TOFMS provides for non-skewed mass spectra making peak deconvolution possible.

Use of a modified QuEChERS sample preparation procedure was fully evaluated for identification and quantitation of pesticides in lettuce using gas chromatography and ion trap mass spectrometry. Final results compared favorably to the reporting and detection limits offered by several worldwide agencies, demonstrating a robust and reliable solution for analyzing pesticide residues in lettuce.

The second unregulated contaminant monitoring regulation (UCMR2) program was developed to monitor US drinking water sources for currently unregulated compounds. EPA Method 527 is categorized under List 1; Assessment Monitoring in the UCMR2 program. EPA Method 527 focuses on a wide range of semi volatile organic contaminants, including pesticides that were deferred during the first UCMR, flame retardants, and pyrethroid pesticides. This application for EPA Method 527 employs SPE with analysis by gas chromatography–mass spectrometry (GC–MS).

Capillary flow technology (CFT) devices are microfluidic components that extend capillary GC capabilities through simple and robust connections between pressure/flow modules and columns. One of the most powerful and simple is the CFT Tee. This is especially useful in GC–MS analysis providing (1) rapid column and inlet maintenance without MSD venting and (2) the capability of rapidly removing late eluting interferences from the column by forcing their retreat into the injection port through "backflushing". Removing these interferences improves column and detector longevity and analytical integrity. Backflushing is very valuable for trace GC–MS analysis in samples from complex matrices like soil, foods or tissues. The CFT Tee uses pressure-pulsed injections and constant flow mode with minimal loss in the MS signal. This approach will be useful to all GC–MS users who want to improve their instrument uptime.

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.

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).

Phthalates are added to plastics to increase flexibility. Recently, concerns have been raised over the effect of phthalate exposure from plastic materials on human health.

By William Goodman, PerkinElmer, Inc.

Contamination of public buildings with PCBs used as softeners in the 1970's in sealants and wall and ceiling paints can still be detected. If certain threshold values in indoor air are exceeded the source has to be decontaminated. This requires an effective and fast determination of the PCB concentration in indoor air. Thermodesorption GC–MS is a method especially suitable for this purpose. Polychlorinated Biphenyls (PCBs) are highly toxic and carcinogenic chemical substances. Although first prepared in 1864, they have been industrially manufactured since 1929. The highest production amounts worldwide were recorded in the 1960s and the beginning of the 1970s. In the 1970s their use as additives for building materials was widespread because of their flame inhibiting and noise reduction properties.

Pesticides are widely used by farmers to control pests, weeds and molds that would otherwise decrease crop production. While this has significantly increased worldwide food productions, these same pesticides pose health risks to humans. The restrictions for specific pesticides differ from one country to the next and as world trade increases, the potential threat to other countries' populations increases. For this reason, pesticides and other food related allergens are currently the subjects of increasing scrutiny and regulation.

The flavours of malt whisky result from a complex blend of long chain esters and alcohols, derived from the distillation products and the composition of the wooden barrels in which the finished product is aged. As shown below, the new VF-WAXms column from Varian, Inc. is ideal for analysing whisky, especially when trace analysis is needed. The column's ultra-low bleed increases sensitivity, extends column life and improves accuracy, even at higher temperatures. In addition, VF-WAXms columns are suitable for use with MS detectors, as the ultra low bleed eliminates interferences and permits more sensitive detection.

A Deans switch, employing Agilent's Capillary Flow Technology, was configured on an Agilent 7890A GC equipped with dual ECD detectors. A method was developed for the analysis of fish oil for PCB contamination. The Deans switch was used to heart cut 7 indicator PCBs (IUPAC Numbers 28, 52, 101, 118, 138, 153 and 180) from the primary DB-XLB column on to a DB-200 column for further separation. Fish oil from a supplement capsule was simply diluted 1:10 in isooctane and injected directly. To prevent carryover, contamination and retention time shifts, the Deans switch was used to backflush the primary column at the end of each run.

AC Analytical Controls developed a new chromatographic solution that complies with all ASTM & EN chromatographic test methods listed in biodiesel specifications: the AC all-in-one Biodiesel analyser. Analysis results demonstrate that the AC analyser complies with EN 14103, EN 14105, EN 14106, EN 14110 & ASTM D6584 methods.

Michael D. Buchanan, Sigma-Aldrich/Supelco

Polycyclic aromatic hydrocarbons (PAHs) are commonly found throughout the environment in soil, water and adsorbed to fine particulate matter in air. Of the 16 common PAHs, 7 have been classified as animal carcinogens by the International Agency for Research on Cancer (IARC). Resulting from this classification, PAHs are monitored and regulated in the environment.

Pesticide contamination of foodstuffs has become a worldwide concern, prompting various levels of regulation and monitoring. Traditionally, pesticides are quantified with gas chromatography (GC) combined with selective detectors (ECD, FID, etc.). Selective GC detectors are great tools to quantify one or two classes at a time. However, screening for a number of different classes of pesticides requires multiple runs utilizing various GC configurations to achieve sufficient chromatographic resolution for unambiguous quantification. Gas chromatography–mass spectrometry (GC–MS) provides positive confirmation of various pesticides in a single analytical run because its superior selectivity allows interference-free quantification even with peak coelution. GC–MS has become a preferred technique for pesticide analysis because of its single-run capability.

The continual increase in sample numbers in busy labs means that it is often difficult for quality control or contract analysis labs to maintain short turnaround times, particularly when instruments are already running at full capacity. To address the need for faster analysis while retaining the quality of separation offered by dedicated amino acid analysers, an improved formulation of sodium citrate based buffers has been developed by Biochrom.

William Goodman and Thomas Meaker, PerkinElmer Life and Analytical Sciences

The analysis of peptides and additives using a new HPLC innovative column technology, Pathfinder, was shown. For the analysis of flavours in lemon juice GC–MS with a new MS library, FFNSC, with linear retention indices was used.

Soft drink formulas often include preservatives, artificial sweeteners, flavours or caffeine in their list of ingredients. Using the Acclaim OA column, as many as eight common additives may be determined in a single run. Many of these additives are hydrophilic organic acids for which this column was designed. Notably, benzoate and sorbate, which do not resolve on C18 columns at low pH, are fully separated.

Column lifetime is a more and more important issue when developing an analytical method for HPLC. Besides sample treatment, column cleaning and storage, operational parameters of the analytical method will have an influence on column lifetime. This question may not always be addressed early enough in the methods development process.