Inge de Dobbeleer, Joachim Gummersbach, Hans-Joachim Huebschmann, Anton Mayer, Paul Silcock Keywords <br>organochlorine pesticides; polychlorinated biphenyls; polycyclic aromatic hydrocarbons; soil samples; water samples; building materials; reproducibility; Results and discussion All test compounds eluted peaks over the course of the 17 minute chromatographic analysis. Chromatographic separations remained stable after more than 100 needles of water, soil and building materials samples were tested. standard curve line Accuracy Test for Adding Matrix Samples <br>The reproducibility tests for three matrices were performed by adding soil extracts, water extracts, and building material extract samples by repeated injection tests. All samples were tested 7 times and the RSD was calculated by external standard method (Table 2). The reproducibility test for all compounds in the matrix was less than 10% RSD. All results were calculated for TraceFinder's automatic integration and were not manually adjusted. Sample Test Results <br> Figure 7 shows the ion chromatographic peaks of a small portion of the compound in a low concentration matrix sample to demonstrate the sensitivity and selectivity of the test method. Conclusions • The TSQ 8000 GC-MS/MS uses a one-stop integrated software tool that greatly simplifies method development, validation and management workflows. references radiopaque adhesive tape,Radiopaque Tape,Medical Tape Anesthesia Medical Co., Ltd. , https://www.jssinoanesthesia.com
Thermo Fisher Scientifc, Dreieich, Germany
Experimental Objectives <br>The gas phase-triple quadrupole tandem mass spectrometry (GC-MS/MS) was used to analyze semi-volatile compounds in various environmental matrices to demonstrate the instrument's test efficiency and corresponding high quality test results.
Foreword
Organochlorine pesticides (OCPs), polycyclic aromatic hydrocarbons (PAHs), and polychlorinated biphenyls (PCBs) are common target analytes in routine environmental analysis laboratories and outsourced testing laboratories. These laboratories have developed a variety of test methods for the analysis of these compounds in various environmental matrices.
Gas-mass spectrometry (GC-MS) is ideal for the analysis of OCPs, PAHs, and PCBs. Environmental analysis laboratory applications compared to conventional detectors such as high performance liquid-ultraviolet fluorescence detectors (HPLC-UVF), gas phase-electron capture detectors (GC-ECD), gas phase-flame ion detectors (GC-FID) Gas phase-single quadrupole mass spectrometry significantly improves the detection sensitivity of such compounds. This effectively simplifies the sample pre-processing steps to a certain extent, improves the analysis efficiency, and reduces the laboratory cost. The test sensitivity of GC-MS/MS is further significantly improved compared to GC-MS.
This greatly increases the instrument's ability to avoid the effects of matrix chemistry (ie, interfering substances), thereby increasing the throughput of environmental analysis laboratories. This technology has been applied by more and more environmental analysis laboratories to enhance its competitiveness. Unfortunately, for laboratories that are just beginning to contact GC-MS/MS instruments, the main challenge in accepting this technology comes from how to achieve high-throughput testing without affecting the continuous operation of the laboratory. 1,2
This application note describes the use of the Thermo ScientificTM TRACETM 1310 Gas Chromatograph in conjunction with the TSQTM 8000 Triple Quadrupole Mass Spectrometer for efficient, high-throughput analysis of OCPs, PAHs, and PCBs in environmental samples. It demonstrates the application of intelligent software tools in the establishment of test methods and data processing processes to minimize the time taken to implement and maintain the entire test process.
Experimental condition
Sample preparation
Water sample
Add n-hexane to the 1L sample and shake to mix. After the aqueous phase and the organic phase were separated, the organic phase was taken and anhydrous sodium sulfate was added to remove water. Each organic phase extract was concentrated by evaporation to 3–4 mL and concentrated to a final volume by evaporation under a gentle stream of nitrogen.
Solid sample
Weigh 10 g of sample (soil, sediment or building material) in a glass container, add anhydrous sodium sulfate and 40 mL of mixed extraction solvent (hexane and acetone). The glass vessel was sealed with Teflon and sonicated for 20 min. A sample extract was placed in a Kuderna-Danish concentrator, and 40 mL of the mixed extraction solvent was added to the precipitate and the above extraction process was repeated. The second extract is combined with the first extract. The extract was concentrated by evaporation to 3–4 mL and concentrated to a final volume by evaporation under a gentle stream of nitrogen.
Method Setup <br>Building a Thermo ScientificTM TRACETM 1310 Gas Chromatograph
Test method: mass spectrometry acquisition and quantification
Experimenters can use the automated SRM method development capabilities in the TSQ 8000 GC-MS/MS system to reduce the time required for method development. AutoSRM can significantly speed up the process of method development. And comprehensive and fast traceability tracking of all parameter optimization processes. In the method development process, all peaks were identified by library search by first-time mass spectrometry. Click on each ion chromatographic peak to find the most abundant ions, and program these ions into the work list and scan them for ion ions during the second injection test.
The test results are also presented in the form of ion chromatograms. By clicking on each chromatographic peak, the corresponding product ions are arranged in a descending order according to relative abundance. Finally, the above ions are programmed into the work list, and the final optimization is performed using the ascending collision energy collision ions. The final optimization results are presented graphically and compiled into the third work list. Use this table to create an SRM method that includes all the compounds, including the complete instrumentation method. In addition, all ion pair information and retention time information can be imported into a compound database and automatically converted to instrument quantification methods using Thermo Scientific TraceFinderTM software.
A full description can be found in the application brief AB52998: Introduction to AutoSRM: Simplifying MRM brings high quality test results. 3
Tuning
The TSQ 8000 GC-MS provides fully automated tuning to ensure reproducible tuning results even when the instrument is operated by different operators. The tuning includes automatic leak detection by applying a certain amount of air to the ion source to check the background ratio of the local air/water.
The tuning results are automatically saved. The most recent tuning file is automatically associated with the instrument method, but the user can still manually change to another tuning file in the instrument method.
Method Reproducibility and Instrument Performance <br> The goal of this establishment and optimization method is to reduce the amount of labor required to analyze a large number of target compounds in the laboratory. To efficiently analyze all target compounds, we optimized the TRACE 1310 Gas Chromatograph and TG-XLBMS column parameters to achieve separation of key isomers.
Standard curves for OCPs and PCBs range from 2 μg/L to 700 μg/L. PAHs require a wider range of quantitation from 2 μg/L to 2500 μg/L. The standard curve was not corrected with an internal standard substance.
The linear correlation coefficients of all standard curves are greater than 0.995. The standard curve for some of the target compounds is shown in Figures 3 and 4.
Minimum limit of quantitation (2 μg/L)
All compounds responded well at the lowest limit of quantitation (2 μg/L or 2 pg on the column) with high signal-to-noise ratio. Figure 5 shows the SRM channel ion chromatogram of some compounds at this concentration point.
The ion chromatograms of some of the low concentration compounds in the matrix samples shown below are labeled as absolute column loadings.
• Combine the three independent methods into one new method, reducing the original three tests to one, effectively increasing the throughput efficiency of the laboratory.
• The overall system has excellent quantitative capabilities and demonstrates good linear regression, ultra-high sensitivity and precision in a range of environmental matrix sample tests.
1. Analysis of emerging persistent organic pollutants using GC-MS/MS; Kalachova et al. SETAC, Berlin 2012.
2. Ziegenhals, K.; Hubschmann, HJ Fast-GC/HRMS toquantify the EU priority PAH. J. Sep. Sci. 2008, 31, 1779 –1786.
3. Thermo Scientific Application Brief AB52998: Introducing AutoSRM: MRM Simplicity for High Performance Results; Cole J.
4. REGULATION (EC) No 2002/657 on analytical performance criteria.
5. Pesticides Method Reference, 2nd ed. 2011, Thermo Fisher Scientific, Austin, TX, USA, P/N 120390.
Analysis of Organochlorine, Polycyclic Aromatic Hydrocarbons and Polychlorinated Biphenyls in Environmental Samples by Gas Phase-Triple Quadrupole Mass Spectrometry>