JEOL Resourceshttps://www.jeolusa.com/RESOURCES/Analytical-Instruments/Documents-DownloadsIdentification of Impurities in an Expired Standard Drug Mixture by Using Multiple Ionization Methods and msFineAnalysishttps://www.jeolusa.com/RESOURCES/Analytical-Instruments/Documents-Downloads/identification-of-impurities-in-an-expired-standard-drug-mixture-by-using-multiple-ionization-methods-and-msfineanalysisAccuTOF™ GCTue, 18 May 2021 15:13:21 GMTGas chromatography combined with high-resolution time-of-flight mass spectrometry (GC-HRTOFMS) is a powerful tool for the analysis of complex mixtures. The AccuTOF GC-Alpha (JMS-T2000GC) mass spectrom-eter is fast, accurate and sensitive with high mass-resolving power and high mass accuracy.<h3>INTRODUCTION</h3> <p>Gas chromatography combined with high-resolution time-of-flight mass spectrometry (GC-HRTOFMS) is a powerful tool for the analysis of complex mixtures. The AccuTOF GC-Alpha (JMS-T2000GC) mass spectrom-eter is fast, accurate and sensitive with high mass-resolving power and high mass accuracy.<br />  </p> <p>Data analysis based on database matching alone does not necessarily provide reliable assignments for com-pounds that have similar electron ionization (EI) mass spectra or compounds that do not have entries in mass spectral databases. JEOL msFineAnalysis software provides automated analysis that makes use of all of the information available from a GC-HRTOFMS analy-sis: elemental composition determination from soft and hard ionization with exact mass measurements and accurate isotope data, database searching, frag-ment ion coverage, and retention index data.</p> <p><br /> In this work, GC-MS analysis of a 12-year-old standard drug mixture was carried out with the AccuTOF GC-Alpha (JEOL JMS-T2000GC) mass spectrometer using the combination electron ionization/photoionization (EI/PI) ion source and the chemical ionization (CI) ion source. Data analysis using JEOL msFineAnalysis software carried out chromatographic deconvolution and identified the drugs and impurities by combining and integrating all of the information from EI and PI analysis.</p> <h3>Please download the application note below to read more.</h3> AccuTOF GC Environment, Food, Flavor, & Fragrance Applications Notebookhttps://www.jeolusa.com/RESOURCES/Analytical-Instruments/Documents-Downloads/accutof-gc-environment-food-flavor-fragrance-applications-notebookMS Product BrochuresThu, 11 Mar 2021 09:52:53 GMTPublication containing various applications pertaining to Environment, Food, Flavor, & Fragrance.<p>Publication containing various applications pertaining to Environment, Food, Flavor, & Fragrance.</p> <h2>Please click below to Download.</h2> Integrated Analysis of Fatty Acid Methyl Esters using msFineAnalysis v2 - MSTips 301https://www.jeolusa.com/RESOURCES/Analytical-Instruments/Documents-Downloads/integrated-analysis-of-fatty-acid-methyl-esters-using-msfineanalysis-version-2AccuTOF™ GCMon, 13 Apr 2020 12:36:36 GMTFatty 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.<h3>Experiment</h3> <p>A commercial 37-component FAMEs standard mixture (Restek, 200-600 ng/μL) was used as a sample. Table 1 shows the measurement conditions used for the GC/EI and GC/FI analyses.</p> <p>Table 1. Measurement conditions</p> <table border="1" cellpadding="1" cellspacing="1" class="table"> <tbody> <tr> <th colspan="2">[GC-TOFMS Conditions]</th> </tr> <tr> <td>System</td> <td>JMS-T200GC (JEOL)</td> </tr> <tr> <td>Ion Source</td> <td>EI/FI combination ion source</td> </tr> <tr> <td>Ionization mode</td> <td>EI+: 70 eV, 300 μA<br /> FI+: -10 kV, 50mA, Slope mode</td> </tr> <tr> <td>Mass Range</td> <td><em>m/z</em> 35-600</td> </tr> <tr> <td>GC column</td> <td>DB-5MSUI, 30 m x 0.25 mm, 0.25 μm</td> </tr> <tr> <td>Oven temp.</td> <td>50°C (1 min) → 10°C/min → 140°C → 3°C/min → 260°C (5 min)</td> </tr> <tr> <td>Inlet mode</td> <td>Split 50:1</td> </tr> </tbody> </table> <h3>Results and discussions</h3> <p>Figure 1 shows the TICC for the GC/EI and GC/FI measurements. While the sample contains 37 components, there were only 36 peaks observed in each chromatogram. The <em>cis</em>-4,7,10,13,16,19-docosahexaenoic acid methyl ester (C<sub>23</sub>H<sub>34</sub>O<sub>2</sub>) and the heneicosanoic acid methyl ester (C<sub>22</sub>H<sub>44</sub>O<sub>2</sub>) coelute with exactly the same retention time (RT) at 38.8 min. However, the FI mass spectrum for this peak showed the molecular ions for each component (Figure 2). Because the JMS-T200GC is always measuring high-resolution mass spectra, these components, which are not quite separated in the chromatogram, can be identified by mass separation.</p> <p><img alt="" class="img-responsive" src="https://jeolusa.s3.amazonaws.com/resources_ai/429/image001.png?AWSAccessKeyId=AKIAQJOI4KIAZPDULHNL&Expires=2145934800&Signature=IxEXbNF3bhbqRM1%2FbFTuuou%2BOhY%3D" /><br /> Figure 1. GC/EI and GC/FI total ion current chromatograms for the  37 FAMEs mixture</p> <p><em><img alt="" class="img-responsive" src="https://jeolusa.s3.amazonaws.com/resources_ai/429/image002.png?AWSAccessKeyId=AKIAQJOI4KIAZPDULHNL&Expires=2145934800&Signature=FowXwdEF9CRCZquBUFuRQu%2F3C2A%3D" /><br /> m/z</em>    Formula    Error<br /> [mDa]    DBE<br /> 340.3329    C<sub>22</sub>H<sub>44</sub>O<sub>2</sub>    -0.7     1.0 <br /> 342.2536    C<sub>23</sub>H<sub>34</sub>O<sub>2</sub>    -1.8     7.0</p> <p>Figure 2. FI mass spectrum (enlarged) at RT 38.8 min and exact mass analysis results</p> <p><img alt="" class="img-responsive" src="https://jeolusa.s3.amazonaws.com/resources_ai/429/image003.png?AWSAccessKeyId=AKIAQJOI4KIAZPDULHNL&Expires=2145934800&Signature=la9LTlh%2B7TXmoIqxZKvrE%2FOvqhg%3D" /><br /> Figure 3. EI and FI mass spectra of 5, 8, 11, 14, 17-eicosapentaenoic acid methyl ester (all-Z)- </p> <p>The FI mass spectra show molecular ions for all 37 FAMEs in the mixture. Additionally, these molecular ions are the base peak in each FI mass spectrum except for the 15-tetracosenoic acid methyl ester (Z)-, which is detected at a relative intensity of >80%. All of these results demonstrate that FI ionizes FAMEs softly and efficiently. As an example, Figure 3 shows the EI and FI mass spectra for 5,8,11,14,17-eicosapentaenoic acid methyl ester (all-Z)-, which has 5 double bonds and an alkyl group. In this example, the molecular ion was not observed in the EI mass spectrum, but the molecular ion is the base peak in the FI mass spectrum. Figure 4 shows the FI mass spectra and chemical formulas for 6 components that all have a carbon number of 20 (minus the ester bond) and have 0 to 5 double bonds. Lastly, Table 2 shows the integrated analysis report generated by msFineAnalysis. In each case, the FI molecular ion accurate masses were automatically used to determine the molecular formula for each component in the FAMES mixture to help identify the correct match from the EI library database search.</p> <p><img alt="" class="img-responsive" src="https://jeolusa.s3.amazonaws.com/resources_ai/429/image004.png?AWSAccessKeyId=AKIAQJOI4KIAZPDULHNL&Expires=2145934800&Signature=8yV1KBB0KRI3msxLjTKDh14pvW4%3D" /><br /> Figure 4. FI mass spectra for the C20 FAMEs </p> <p>Table 2. Integrated qualitative analysis results report using msFineAnalysis<br /> <img alt="" class="img-responsive" src="https://jeolusa.s3.amazonaws.com/resources_ai/429/image005.png?AWSAccessKeyId=AKIAQJOI4KIAZPDULHNL&Expires=2145934800&Signature=dBTZBLAt1O%2FNuS1vBHFgYlI5kJY%3D" /></p> <h3>Conclusions</h3> <p>The msFineAnalysis integrated analysis method produces highly accurate qualitative analysis results for the FAMEs by combining the library search results and molecular formula estimation. This combination of using GC/EI and GC/FI measurements together for qualitative analysis is particularly important for FAMEs as these types of compounds do not produce molecular ions for EI, making it difficult to use database searches alone for identification.</p> SPME-GCxGC/HRTOFMS Analysis of Tequilahttps://www.jeolusa.com/RESOURCES/Analytical-Instruments/Documents-Downloads/spme-gcxgchrtofms-analysis-of-tequilaMass Spectrometry (MS)Thu, 05 Mar 2020 08:26:18 GMTThe JEOL “AccuTOF GCv 4G” is a third generation GC/HRTOFMS system with high speed data acquisition capabilities of up to 50Hz which makes it well suited as the detector for comprehensive 2-dimensional GC (GCxGC) measurements. Along with the high speed data acquisition, this MS system also provides high mass resolution, accurate mass measurements, and high sensitivity, all simultaneously. Consequently, this GCxGC/HRTOFMS system is a powerful tool for the qualitative analysis of complicated samples. In this work, we measured commercially available tequila samples using GCxGC/HRTOFMS combined with solid-phase micro-extraction (SPME) preparation.<p>In this work, we measured commercially available tequila samples using GCxGC/HRTOFMS combined with solid-phase micro-extraction (SPME) preparation.</p> Quantitative Analysis of Pyrazole Pesticides in Tea Leaf by Using FastGC-HRTOFMShttps://www.jeolusa.com/RESOURCES/Analytical-Instruments/Documents-Downloads/quantitative-analysis-of-pyrazole-pesticides-in-tea-leaf-by-using-fastgc-hrtofmsMass Spectrometry (MS)Thu, 05 Mar 2020 08:19:30 GMTThe FastGC method is a very useful technique for doing rapid GC analyses that result in extremely narrow chromatographic peaks over a shorter time period than traditional GC analyses. Additionally, time-of-flight mass spectrometers (TOFMS) are capable of very fast data acquisition in comparison with other types of mass spectrometers so they are well suited as the detector for the FastGC technique. Furthermore, when the TOFMS is capable of high resolution measurements, the resulting mass spectra contain accurate mass information that can be used to calculate the elemental compositions for each observed m/z. In this application note, we describe the quanitative analysis of pyrazole pesticides (Fipronil, Ethiprole, Pyraflufen ethyl and Tebfenpyrad) on tea leaves by FastGC/HRTOFMS. Additionally, we confirm that a rapid analysis with high sensitivity is easy to perform and very useful for fast screening.<h3>Method</h3> <p>The tea leaf sample (5g) was prepared using the multiresidue method for agricultural chemicals by GC/MS published by Ministry of Health, Labour and Welfare, Japan. The pyrazole pesticides were added to make 0.01, 0.05 and 0.1ppm solution in the prepared solution from tea leaf. These concentrations in solution are equivalent to 4, 20 and 40ppb in tea leaf. Each sample was analyzed 3 times to check the reproducibility of the results.</p> Qualitative Analysis of Pyrazole Pesticides in Tea Leaf by Using FastGC-HRTOFMShttps://www.jeolusa.com/RESOURCES/Analytical-Instruments/Documents-Downloads/qualitative-analysis-of-pyrazole-pesticides-in-tea-leaf-by-using-fastgc-hrtofmsMass Spectrometry (MS)Thu, 05 Mar 2020 08:16:25 GMTThe FastGC method is a very useful technique for doing rapid GC analyses that result in extremely narrow chromatographic peaks over a shorter time period than traditional GC analyses. Additionally, time-of-flight mass spectrometers (TOFMS) are capable of very fast data acquisition in comparison with other types of mass spectrometers so they are well suited as the detector for the FastGC technique. Furthermore, when the TOFMS is capable of high resolution measurements, the resulting mass spectra contain accurate mass information that can be used to calculate the elemental compositions for each observed m/z. In this application note, we describe the qualitative analysis of pyrazole pesticides (Fipronil, Ethiprole, Pyraflufen ethyl and Tebfenpyrad) on tea leaves by FastGC/HRTOFMS. Additionally, we confirm that a rapid analysis with high sensitivity is easy to perform and very useful for fast screening.<h3>Method</h3> <p>The tea leaf sample (5g) was prepared using the multiresidue method for agricultural chemicals by GC/MS published by Ministry of Health, Labour and Welfare, Japan. Pyrozole pesticides were added to make 0.01, 0.05 and 0.1ppm solutions in the prepared solution from tea leaf. These concentrations are equivalent to 4, 20 and 40ppb on the tea leaf material. Each sample was then analyzed 3 times to check the reproducibility of the results.</p> Qualitative Analysis by Comprehensive 2D GC / TOFMS[2]: Analysis of polycyclic aromatic hydrocarbons in kerosenehttps://www.jeolusa.com/RESOURCES/Analytical-Instruments/Documents-Downloads/qualitative-analysis-by-comprehensive-2d-gc-tofms2-analysis-of-polycyclic-aromatic-hydrocarbons-in-keroseneMass Spectrometry (MS)Thu, 05 Mar 2020 08:13:58 GMTComprehensive two-dimensional gas chromatography (GC×GC) is a kind of continuous heart-cut GC system. Two different types of columns are connected via a modulator in the same GC oven. By using the two columns together, this technique provides very high separation capabilities when compared to one- dimensional GC analysis. However, GC×GC systems require a fast data acquisition detection system in order to record the very narrow time width peaks observed in the GC chromatograms. The JEOL AccuTOF-GC is a time-of-flight mass spectrometer (TOFMS) that fully meets this high speed data acquisition requirement at 25Hz (0.04sec) so it can be successfully used as the detection system in combination with GC×GC. In this work, the AccuTOF-GC was used for the qualitative analysis of polycyclic aromatic hydrocarbons in kerosene by GC×GC -TOFMS.<h3>Results and Discussion</h3> <p>All of the chromatograms were created by using the Zoex GC Image software. The GC×GC 2D and 3D chromatograms for kerosene are shown in Fig.1. The X-axis corresponds with the separation by the 1<sup>st</sup> column which is based on differences in boiling point, and the Y-axis corresponds with the separation by the 2<sup>nd</sup> column which is based on differences in polarity. Also, the colors in the chromatograms show the intensity of each peak. The intensity increases from light blue to yellow to red. The red color shows that the compound intensity is over the settings value for the maximum intensity.</p> Examining Selectivity by Using High Resolution Mass Chromatographyhttps://www.jeolusa.com/RESOURCES/Analytical-Instruments/Documents-Downloads/examining-selectivity-by-using-high-resolution-mass-chromatographyMass Spectrometry (MS)Wed, 04 Mar 2020 19:36:25 GMTTransformer oil containing no PCBs was diluted 10,000 times, and then this solution was spiked with a mixture of commercially available PCBs (KC-500). The resulting sample was analyzed by using the JEOL AccuTOF-GC with FastGC/MS conditions. Afterwards, the data was examined by varying the mass range window (called "window width") used for the PCB reconstructed ion chromatogram (RIC) to determine if the effect of the background impurities can be eliminated so that the analyte peaks are easily observed in the resulting data.<h3>Introduction</h3> <p>Transformer oil containing no PCBs was diluted 10,000 times, and then this solution was spiked with a mixture of commercially available PCBs (KC-500). The resulting sample was analyzed by using the JEOL AccuTOF-GC with FastGC/MS conditions. Afterwards, the data was examined by varying the mass range window (called "window width") used for the PCB reconstructed ion chromatogram (RIC) to determine if the effect of the background impurities can be eliminated so that the analyte peaks are easily observed in the resulting data.</p> Determination of Triazolam by AccuTOF™ GC/Time-of-Flight Mass Spectrometryhttps://www.jeolusa.com/RESOURCES/Analytical-Instruments/Documents-Downloads/determination-of-triazolam-by-accutof-gctime-of-flight-mass-spectrometryMass Spectrometry (MS)Wed, 04 Mar 2020 19:32:10 GMTTriazolam is a benzodiazepine with a very short elimination half-life. The range is reported to be 1.5 to 5.5 hours. Due to its frequent use as a sedative and its potential to affect human activities such as driving, an unambiguous and sensitive analysis method is needed for its identification and quantitation. Generally, for determination of triazolam, screen tests are performed in biological samples followed by confirmation and quantitation with GC/MS. Here, we demonstrate the feasibility by using the JEOL AccuTOF™ GC, time-of-flight mass spectrometer with accurate mass measurement and negative ion chemical ionization (NCI) capabilities for triazolam determination. D4-triazolam was used as internal standard. The mass accuracy without internal reference is smaller than 2 mmu. The limit of detection is 5 ng/mL. The quantitation standard curve can be linear from 5 ng/mL to 1000 ng/mL with R2 of 0.9992. To the best of our knowledge, this is the first time that triazolam has been detected by GC/time-of-flight mass spectrometry with accurate mass measurement.<h3>Introduction</h3> <p>Triazolam is a benzodiazepine with a very short elimination half-life. The range is reported to be 1.5 to 5.5 hours. Due to its frequent use as a sedative and its potential to affect human activities such as driving, an unambiguous and sensitive analysis method is needed for its identification and quantitation. Generally, for determination of triazolam, screen tests are performed in biological samples followed by confirmation and quantitation with GC/MS. Here, we demonstrate the feasibility by using the JEOL AccuTOF™ GC, time-of-flight mass spectrometer with accurate mass measurement and negative ion chemical ionization (NCI) capabilities for triazolam determination. D4-triazolam was used as internal standard. The mass accuracy without internal reference is smaller than 2 mmu. The limit of detection is 5 ng/mL. The quantitation standard curve can be linear from 5 ng/mL to 1000 ng/mL with R<sup>2</sup> of 0.9992. To the best of our knowledge, this is the first time that triazolam has been detected by GC/time-of-flight mass spectrometry with accurate mass measurement.</p> Comprehensive Analysis + Unknown Component Analysis of Coffee Samples Using Headspace GC-MShttps://www.jeolusa.com/RESOURCES/Analytical-Instruments/Documents-Downloads/comprehensive-analysis-unknown-component-analysis-of-coffee-samples-using-headspace-gc-msMass Spectrometry (MS)Wed, 04 Mar 2020 19:24:24 GMTAdvances in mass spectrometry are enabling analysis of micro samples and unknown components that were not observable before. As the volume of information acquired from mass spectrometry increases, researchers are calling for simple techniques to analyze numerous components observed, and as a result, there is a rise in demand for comprehensive analytical techniques including multiple classification analysis. In this work, we will introduce a new technique of non-targeted analysis, which combines comprehensive analysis using high resolution GC-MS and unknown component analysis using soft ionization and EI.<h3>Experiment</h3> <p>Table 1 shows the measurement conditions. Four different types of commercial coffee (A: Indonesian; B: Ethiopian; C: Guatemalan; D: Brazilian) were selected as samples. Each sample was measured 5 times (n=5).</p>