Application Notes

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.

Calvados is an apple-brandy of Normandy (France). Mashed apples are fermented to obtain cider and then distilled to give the young spirit.

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.

Multidimensional liquid chromatography (MDLC) techniques are essential for the separation of highly complex proteomic samples. Advantages of off-line MDLC techniques over on-line approaches include high flexibility in choice of column dimensions and mobile-phase compositions, and the ability to reanalyse sample fractions. Here we present a fully automated off-line two-dimensional chromatographic approach for the analysis of proteomic samples using an UltiMate 3000 system optimized for proteomics MDLC.

Combining an ultra fast LC system (e.g., Agilent 1200RRLC, Waters UPLC) with an accurate mass TOF mass spectrometer creates a powerful system for information-rich high-throughput analyses. However, for de novo formula generation and confirmation the residual mass accuracy tolerance of 3–5 ppm can still leave significant ambiguity in the proposed formula. Consequently, skilled manual inspection or further measurements deploying additional analytical techniques (NMR or MS–MS) are frequently required to arrive at a confident formula assignment.

Using ACQUITY UPLC technology with triple quadrupole MS detection enhances the selectivity, sensitivity and throughput in quantitative bioanalytical studies. Detection limits for these methods are being driven lower and lower as drugs become more potent.

The pyrolysis fragments are first refocused on the top of the GC column, then separated and finally detected by the MS. At the end of the GC run the SEC flow is resumed again and the entire process is repeated.

Calvados is an apple-brandy of Normandy (France). Mashed apples are fermented to obtain cider, which is then distilled to give the young spirit.

The process of investigating a suspicious fire includes many different types of analyses. An essential step in confirming the presence of a liquid accelerant is gas chromatography (GC); detection with a mass spectrometer (MS) provides an accurate confirmation of both the presence and identity of an accelerant. In arson analysis, the sample preparation for GC–MS analysis is typically performed by headspace or solvent extraction.

PLOT columns are often used in GC analyses when it is necessary or desirable to retain one class of solutes in favour of other solutes that have little or limited interactions with the surface of the stationary phase. With a PLOT column, chromatographers can even cause lower boiling point compounds to elute well after higher boiling point compounds, thus providing better qualitative and quantitative separations for the solutes of interest.

This article describes a fully automated online solid-phase extraction–liquid chromatography–tandem mass spectrometry (SPE–LC–MS-MS) setup using a mass spectrometer and an electrospray ionization probe for analyzing different groups of polar contaminants in natural waters. The goal was to develop an online SPE method for the quantification of sulfonamide antibiotics, including their acetyl metabolites, as well as for frequently used pesticides (triketones, phenylureas, chloracetanilides, phenoxyacetic acids, amides, and triazines) in ambient waters. The analytical methods were applied successfully for a field study in an agricultural region within the catchment area of Lake Greifensee near Zurich, Switzerland.

Drug discovery scientists are continually striving to improve productivity and efficiency in their workflows. From early discovery to clinical development, existing workflow bottlenecks represent an opportunity to develop solutions to speed the process and improve productivity. The key requirements for quantitative analysis are precision, accuracy, and linear dynamic range. With any quantitative instrument, the hope is that it will be applicable to a vast range of coumpounds, ruggest, and fast. New mass spectrometry (MS) technologies are being developed that meet these criteria and permit high throughput while enabling its application to areas in which speed limitations previously curtailed its practicality. In particular, in the area of ADME profiling, new MS platforms are becoming available that increase the throughput by at least 25-fold, by combining the speed of matrix-assisted laser desorption ionization (MALDI) with the specificity of triple-quadrupole MS. This is bound to greatly accelerate the ADME..

Root diseases caused by soilborne plant pathogens are responsible for billions of dollars of losses annually in food, fiber, ornamental, and biofuel crops. The use of pesticides often is not an option to control plant diseases because of economic factors or potential adverse effects on the environment or human health. For this reason, many Americans are now buying pesticide-free organic foods. Organic agriculture has few options for controlling pests and thus must make full use of natural microbial biological control agents in soils that suppress diseases.

Mass spectrometry (MS) has advanced to analyze ever-larger biomolecules with the invention of soft ionization techniques like electrospray ionization (ESI). Although ESI has provided a method of generating ions of high mass, mass spectrometers generally suffer both lower sensitivity and lower resolution as the mass-to-charge ratio of an ion increases. To extend the mass range of ionized macromolecules beyond the limits of MS, macroion mobility spectrometry utilizes ion mobility sizing to characterize charge-reduced ESI-generated macroions from >5 kDa to beyond megadalton masses. One prominent application of macroion mobility spectrometry, highlighted here, is the high sensitivity analysis of intact proteins, antibodies, and conjugates in which molecular masses range from antibody light-chain fragments to high mass immunoglobulin multimers.

Semiquantitative elemental analysis by ICP-MS is a powerful tool for quick screening of unknown samples for a wide range of elements.

Mass spectrometry has become a fundamental tool for compound identification or confirmation by virtue of its ability to obtain elemental composition determination (formula identification) by accurate mass measurements. The speed, sensitivity, and ease of interfacing the technique with gas chromatography and liquid chromatography make it the technique of choice for many applications. However, accurate mass measurements must be made with care, and sometimes they can require careful calibration procedures and validation methods. In addition to accurate mass measurements, the isotope abundance distribution also provides information unique to a given chemical formula. However, the mass spectral accuracy required for accurate isotope modeling has not been easy to obtain previously. More recent approaches (1–3) that calibrate the spectral line-shape show promise in obtaining the necessary level of spectral accuracy but still require careful calibration methods with the use of known standards. This article..

This report shows the steps involved in the development of a new polymethyl methacrylate (PMMA) calibration standard for polar organic GPC applications.

This application note describes an LC–MS–MS method for on-line sample preparation and concentration of drinking water samples prior to analysis using a triple quadrupole with full scan Q3 confirmation.

One problem frequently encountered in LC–MS is the appearance of mass peaks, which appear totally unrelated to the samples run - "ghost" mass peaks. It is impossible to differentiate whether these signals come from an unknown component in the sample co-eluting with a known peak, or from an impurity in the mobile phase or from some residual contamination "bleeding" from the column.

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.

Preliminary studies of biodiesel samples by a high speed LC–MS system using electrospray ionization and a patented cone-wash feature demonstrate that LC–MS reduces the analysis time to 20 minutes and reveals information about higher molecular weight compounds in biodiesel while still detecting many low molecular weight chemicals, including FAMEs, at high sensitivity.

The use of 30 mm UPLC columns coupled with Oasis SPE in µElution format was investigated to increase the speed of quantitative bioanalytical methods while maintaining sensitivity and resolution of closely related analytes.

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.

The effect of switching between high and low pH mobile phases on a single analytical HPLC column was investigated. The ability to rapidly switch between pH extremes on XBridge columns without special washing/re-equilibration steps dramatically reduces the time for separation of pharmaceutical compounds.

The performance of lubricating oil is significantly degraded by the presence of fuel contaminants such as gasoline and diesel. Recycled oil is particularly susceptible to this form of contamination. Consequently, producers and distributors of lubricating oil must go to great lengths to ensure the levels of fuel contamination are kept to a safe limit (typically 4–5%) in these products.

The analysis of crude oil by means of different atmospheric pressure ionization (API) techniques is described. Crude oil is analysed without any separation prior to API-Fourier transform mass spectrometry. The use of a quadrupole/hexapole device to selectively enhance a certain mass range is demonstrated. Automated generation of molecular formulas from accurate mass measurements enables rapid compound identification.

Solid-phase extraction (SPE) has revolutionized sample preparation. Variations on the technique offer enhanced recovery, greater speciation and reduced solvent and sample consumption over other techniques. Micro-extraction packed sorbent (MEPS) is the miniaturization of conventional SPE from millilitre to microlitre bed volumes that allows SPE to be used with very small samples. The manipulation of the small volumes is achieved with a precision gas tight syringe. With a typical void volume of 7 μL, the volume of solvent eluted from MEPS is compatible with GC and LC inlets making it ideal for integration into an automated sampling system for on-line SPE.