Analytical Instrument Documents

Cocoa butter is the edible fat extracted from cocoa beans that is used in the manufacture of chocolate. Cocoa Butter Equivalents (CBE) are a substance derived from palm oil and shea butter that are used as a substitute for cocoa butter in chocolate. European regulations govern the labeling of chocolate as containing CBE less than 5%. US regulations require that Cocoa Butter Equivalents be specifically labeled with wording such as “chocolate flavored” coating. Analysis of the triglyceride content of chocolate is a quality control measure. Analysis of a standard sample of cocoa butter triglycerides is presented here as an example of the use of the JEOL Q1500 quadrupole GC-MS system for the detection of lipids separated by using a high-temperature GC column (Restek Rtx-65TG).

Fatty acid methyl esters (FAMEs) are crucial for determining the fat content in food. Being environmentally friendly, they are also increasingly used as bio-diesel fuels. Many of the FAMEs are unsaturated with double bonds in the alkyl chains. As the number of double bonds increases (more unsaturation), the EI measurements tend to lack molecular ions. In this work, we measured a standard sample containing multiple FAMEs using EI and FI to detect their molecular ions. The resulting data was further examined by using msFineAnalysis to produce an integrated report for these compounds in which the library database search was combined with the molecular ion exact mass analysis to produce a qualitative identification of these compounds.

Electron ionization (EI) is a hard ionization method that is commonly used with gas chromatography mass spectrometry (GC-MS). The mass spectral fragmentation patterns produced by EI are used for library database searches to identify compounds. Conversely, soft ionization methods like field ionization (FI) tend to produce clear molecular ions with minimal fragmentation. When high-resolution MS is used with these ionization techniques, the accurate masses for the fragment ions produced by EI and the molecular ions produced by soft ionization provide an additional dimension of information for the analytes. Combining the exact mass information with the results of conventional library search can enhance the accuracy of identification compared to the use of library search alone.  In this work, we introduce the msFineAnalysis software and use it to automatically combine data acquired by GC/EI and GC/soft ionization for the qualitative analysis of coffee headspace.

In 2018, msFineAnalysis Ver.1 software was released in which data acquired by EI, soft ionization, and accurate mass measurements were automatically integrated to generate a qualitative report for samples measured by these techniques with GC-MS. Recently, msFineAnalysis Ver.2 was introduced as an enhanced version with additional features. In this work, we will describe the changes in Ver.2, which now includes chromatographic deconvolution, and present applications using the new features.

In 2018, we announced the msFineAnalysis software which was designed to automatically integrate two types of data acquired by EI and soft ionization. Recently, we developed msFineAnalysis Version 2, an enhanced version with additional features. msFineAnalysis Version 2 incorporates two new features: Chromatographic Deconvolution and Group Analysis. In this work, we use the group analysis capabilities of the software to evaluate the pyrolysis GC-MS results for a vinyl acetate resin.

JEOL msPrimo and Escrime software provide all of the tools needed to develop optimized methods for target compound quantitation and report generation. In this application note, we describe a sensitive method for analyzing pesticides in Cannabis sativa matrix using the SRM capabilities of our triple quadrupole system.

The chemical composition of herbs and spices can vary dramatically between different species and different growing conditions. Herbs grown under different conditions that have different essential oil compositions are referred to as chemotypes. Basil is an herb that has widely varying chemotypes. The difference between basil leaves from two different sources was easily observed by using DART. A leaf from a basil plant purchased at a grocery store was compared with a leaf from a Vietnamese restaurant. A small particle from each leaf was analyzed placed in front of the DART source. Mass spectra were obtained within seconds. Elemental compositions were confirmed by exact masses and accurate isotopic abundance measurements.

Mass Spectrometry (MS) is one of the fastest-growing areas in analytical instrumentation. The use of mass spectrometry in support of synthetic, organic, and pharmaceutical chemistry is well established. Mass spectrometry is also used in materials science, environmental research, and forensic chemistry. It has also evolved into one of the core methods used in biotechnology. However, currently available ion sources place extreme restrictions on the speed and convenience of sample analysis by mass spectrometry. Here we report a method for using mass spectrometry to instantaneously analyze gases, liquids, and solids in open air at ground potential under ambient conditions. Traditional ion sources used in mass spectrometry require the introduction of samples into a high vacuum system.

Comprehensive two-dimensional gas chromatography (GC×GC) and high-resolution mass spectrometry (HRMS) offer the best possible separation of their respective techniques. Recent commercialization of combined GC×GC–HRMS systems offers new possibilities for the analysis of complex mixtures. However, such experiments yield enormous data sets that require new informatics tools to facilitate the interpretation of the rich information content. This study reports on the analysis of dust obtained from an electronics recycling facility by using GC×GC in combination with a new high-resolution time-of-flight (TOF) mass spectrometer. New software tools for (non-traditional) Kendrick mass defect analysis were developed in this research and greatly aided in the identification of compounds containing chlorine and bromine, elements that feature in most persistent organic pollutants (POPs). In essence, the mass defect plot serves as a visual aid from which halogenated compounds are recognizable on the basis of their mass defect and isotope patterns. Mass chromatograms were generated based on specific ions identified in the plots as well as region of the plot predominantly occupied by halogenated contaminants. Tentative identification was aided by database searches, complementary electron-capture negative ionization experiments and elemental composition determinations from the exact mass data. These included known and emerging flame retardants, such as polybrominated diphenyl ethers (PBDEs), hexabromobenzene, tetrabromo bisphenol A and tris (1-chloro-2-propyl) phosphate (TCPP), as well as other legacy contaminants such as polychlorinated biphenyls (PCBs) and polychlorinated terphenyls (PCTs).

The characterization of organic mixtures by comprehensive two-dimensional gas chromatography (GC×GC) coupled to electron impact (EI) ionization time-of-flight mass spectrometry (TOF-MS) allows the detection of thousands of compounds. However, owing to the exhaustive fragmentation following EI ionization, despite the use of mass spectral libraries, a majority of the compounds remains unidentified because of the lack of parent ion preservation. Thus, soft-ionization energies leading to organic compounds being ionized with limited or no fragmentation, retaining the molecular ion, has been of interest for many years. In this study, photoionization (PI) was evaluated as the ion source for GC×GC-TOF-MS measurements. First, capabilities and limitations of PI were tested using an authentic mixture of compounds of several chemical classes. Ionization energy exhibited by PI, equivalent to 10.8 eV, resulted in significant retention of molecular ion information; [M]+• for alkanes, ketones, FAMEs, aromatics, [M–H]+• for chloroalkanes, and [M–H2O]+• for alcohols. Second, considering the potential of PI for hydrocarbons, base oils, complex mixtures of saturated and unsaturated hydrocarbons blended for finished lubricant formulations, were extensively evaluated. Several chemical classes of hydrocarbons were positively identified including a large number of isomeric compounds, both aliphatics and cyclics. Interestingly, branched-alkanes were ionized with lower excess internal energy, not only retaining the molecular ions but also exhibiting unique fragmentation patterns. The results presented herein offer a unique perspective into the detailed molecular characterization of base oils. Such unprecedented identification power of PI coupled with GC×GC-TOF-MS is the first report covering volatiles to low-volatile organic mixtures.