Plasma deuterium oxide (2H2O) enrichment analysis was performed using a modified acetone equilibration [74 (link)]. Briefly, water was distilled from 100μl aliquots of plasma or saliva in inverted microvials placed in a 70°C glass bead bath. The collected distillate was reacted with 5μl acetone and 1μl 10N NaOH, and left at room temperature for 18–24 hours. Acetone was extracted from treated samples using 300ul hexane and, after drying hexane extracts with Na2SO4 crystals, acetone was analyzed by gas chromatography/mass spectrometry (GC/MS). A standard curve of percent enrichment was prepared gravimetrically from 100% enriched 2H2O. GC/MS analysis of acetone was performed by quadrupole gas chromatography/mass spectrometry (Agilent 6890/5973) using electron impact ionization mode and SIM ions of m/z 58.2 and 58.3 for acetone M0 and M+1. The column used was a DB-17MS, 30M x 0.25mm I.D., 0.25μm film thickness (J&W Scientific, Agilent).
Db 17m
Manufactured by Agilent Technologies
The DB-17MS is a capillary column designed for gas chromatography applications. It features a 30 meter length, 0.25 millimeter internal diameter, and a 0.25 micrometer film thickness. The stationary phase is composed of a 50% phenyl - 50% methylpolysiloxane material.
Automatically generated - may contain errors
Lab products found in correlation
Unity 2 thermal desorber, by Markes International (2 mentions)
Pegasus 4d gc, by Agilent Technologies (2 mentions)
Agilent 6890 gas chromatograph, by Agilent Technologies (2 mentions)
Rtx 5ms, by Restek (2 mentions)
Pegasus 4d tof ms mass spectrometer, by Leco (1 mentions)
Db wax column, by Agilent Technologies (1 mentions)
5 protocols using db 17m
1
Plasma Deuterium Oxide Enrichment Analysis
2
Metabolite Profiling Using GC-TOFMS
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Identification and quantification of metabolites was performed using an Agilent 7890A GC device (Agilent) and a Pegasus 4D TOF/MS mass spectrometer (Leco Corporation, St. Joseph, MI). An Agilent DB-WAX column (30 m × 250 μm × 0.25 μm) was used for all analysis. The temperature program was as follows: 40°C for 3 min; 5°C/min to 250°C; 250°C for 5 min; helium (99.9999%) 1.0 mL/min. Injections were made in splitless mode. A 2-dimensional column was used (DB-17 MS; Agilent), with dimensions of 2 m × 100 μm × 0.10 μm, and an initial column temperature of 255°C. The offset temperature of the secondary GC oven was set at +5°C relative to the temperature of the primary GC oven. Remaining settings were as follows: modulation period: 6.0 s; interface temperature: 270°C; ion source: 250°C; electron impact: 70 eV; detector voltage: 1,680 V; acquisition rate: 50 spectra/s; scan range: m/z 33 to 500; mass spectral library: NIST.
GC-TOFMS analysis of 2 μL extracts was conducted. Volatile components were detected based on the data processing system of MassLynx V4.1 Chemical Workstation, Nist2008, and WILYL standard spectrum libraries, and spectrum analyses from the related literature. Quantitative analysis was conducted using the area normalization method, and the relative percentage contents of volatile components were obtained.
GC-TOFMS analysis of 2 μL extracts was conducted. Volatile components were detected based on the data processing system of MassLynx V4.1 Chemical Workstation, Nist2008, and WILYL standard spectrum libraries, and spectrum analyses from the related literature. Quantitative analysis was conducted using the area normalization method, and the relative percentage contents of volatile components were obtained.
3
Quantitative PAH Analysis in Rubber Toys
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Sample preparation was done according to method AfPS GS 2019:01 PAK. Each step of the sample preparation was performed in a gravimetrically controlled manner, even though volumes are given below. 0.5 g of the rubber toy sample was weighed into a 40-mL screw-capped glass vial. After addition of 20 mL of toluene, the sample was extracted by ultrasonication (PTIC-X-ES, Allpax, Papenburg, Germany) at 60 °C for 1 h. After the extract cooled to room temperature, an aliquot of 0.5 mL was transferred to a 1.5-mL HPLC vial. To this extract aliquot, 100 µL of a deuterated internal standard solution (ISTD) was added and subsequently analyzed by GC–MS system A (Table 1 ).
Instrumental parameters of the two GC–MS systems A and B used for PAH analysis of BAM-B001
| Instrumental parameter | GC–MS system A | GC–MS system B |
|---|---|---|
| GC system | 6890 N (Agilent) + KAS 4 (Gerstel) | 7890A (Agilent) |
| Column | Select PAH (Agilent) | DB-17 ms (Agilent) |
| Column dimensions | 30 m × 0.25 mm × 0.15 µm ID | 60 m × 0.25 mm × 0.25 µm ID |
| Oven program | 70 °C (1 min) → (85 °C/min) 180 °C → (3 °C/min) 230 °C (7 min) → (28 °C/min) 280 °C (10 min) → (14 °C/min) 350 °C (3 min) | 80 °C (1 min) → (5 °C /min) 320 °C (33 min) |
| Carrier gas | He 5.0 (2 mL/min) | He 5.0 (2 mL/min) |
| Injection | 5 µL (large volume injection, LVI) | 1 µL (splitless at 320 °C) |
| MS system | MSD 5975B inert XL (Agilent) | MSD 5975C inert XL (Agilent) |
| Ionization | 70 eV (EI) | 70 eV (EI) |
| Acquisition mode | SIM | SIM |
4
GC-MS Analysis of Volatile Compounds
5
GC-MS Analysis of Volatile Compounds
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Sample tubes were thermally desorbed using a Unity 2 thermal desorber (Markes International Inc., Gold River, CA) onto a Pegasus 4D GC × GC-TOF MS system equipped with an Agilent 6890 gas chromatograph (Agilent Technologies, Santa Clara, CA) in line with a LECO time-of-flight mass spectrometer (LECO Corp, St Joseph, MI). Primary column was a 30 m × 0.25 mm i.d. × 0.25 μm df Rtx-5MS (Restek Corp., Belefonte, PA) and secondary column a 2 m × 0.18 mm i.d. × 0.18 μm df DB-17M (Agilent Technologies, Santa Clara, CA). Carrier gas was helium and runs were performed in splitless mode. The initial temperature was 35 °C for 1 min, followed by ramping to 100 °C at a rate of 5 °C min−1 and ramping to 250 °C at a rate of 8 °C min−1 followed by a 30 s hold. Secondary column and modulator temperature offsets were each set to +20 °C. The thermal modulation periods were set to 5 s, hot pulse time 1 s and cool time between stages 1.5 s. Column flow was set to 2.0 ml min−1 and the total run time was set to 34 min. The transfer line was set to 280 °C and ion source 200 °C. Acquisition rate was set to 200 spectra s−1 with a 120 s delay and mass range of 35–400 amu.
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