Metabolomics Workbench : NIH Data Repository

MB Sample ID: SA167401

Local Sample ID:	BL_200220_M393_389
Subject ID:	SU001878
Subject Type:	Human
Subject Species:	Homo sapiens
Taxonomy ID:	9606

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Subject:

Subject ID:	SU001878
Subject Type:	Human
Subject Species:	Homo sapiens
Taxonomy ID:	9606

Factors:

Local Sample ID	MB Sample ID	Factor Level ID	Level Value	Factor Name
BL_200220_M393_389	SA167401	FL019911	Plasma	type

Collection:

Collection ID:	CO001871
Collection Summary:	200 µL ethylenediaminetetraacetic acid (EDTA)-treated plasma samples were collected following standard operating procedures from 80 individuals without known disease and were randomly selected from archival samples obtained from the Center for Health Discovery and Well Being (CHDWB) cohort of approximately 750 individuals. The original study was conducted under Emory Investigational Review Board (IRB approval No. 00007243) and included both genders and individuals self-identifying as white, black, Hispanic and Asian. SRM-1957 and SRM-1958 were obtained from National Institute of Standard and Technology (NIST) as quality control and assurance measures run in parallel to study samples.
Sample Type:	Blood (plasma)

Treatment:

Treatment ID:	TR001891
Treatment Summary:	50 µL formic acid (Emprove® Essential DAC, Sigma-Aldrich) was added to 200 µL SRM aliquots and immediately followed by addition of 200 µL hexane – ethyl acetate (2:1 v/v, ≥99% pure, Sigma-Aldrich) containing the internal standards (final concentration: 1 ng/mL). The sample mixture was shaken vigorously on ice using multi-tube vortexer (VWR VX-2500) for 1 h and centrifuged at 1000 g, 4 °C for 10 min. The sample mixture was chilled during entire extraction procedure. The organic supernatant was transferred to a new tube with 25 mg MgSO4 (≥99.99% pure, Sigma-Aldrich) and vortexed vigorously to remove water. After 10 min centrifugation at 1000 g, 80 µL of the final supernatant was spiked with instrumental internal standards (final concentration: 1 ng/mL) for analysis. Two 13C labeled chemicals [13C12]PCB-28 and [13C12]PBB-153 were used as volumetric internal standards added to the final extract, and nine 13C labeled chemicals (99% isotope enrichment for each) were spiked as recovery standards to estimate chemical recovery efficiency by XLE: [13C12]PCB-101, [13C12]PCB-153, [13C12]PCB-180, [13C12]PBDE-47, [13C12]PBDE-99, [13C6]anthracene, [13C10]mirex, [13C6]cis-permethrin, and [13C12]p,p’-DDE.

Treatment ID:

TR001891

Treatment Summary:

50 µL formic acid (Emprove® Essential DAC, Sigma-Aldrich) was added to 200 µL SRM aliquots and immediately followed by addition of 200 µL hexane – ethyl acetate (2:1 v/v, ≥99% pure, Sigma-Aldrich) containing the internal standards (final concentration: 1 ng/mL). The sample mixture was shaken vigorously on ice using multi-tube vortexer (VWR VX-2500) for 1 h and centrifuged at 1000 g, 4 °C for 10 min. The sample mixture was chilled during entire extraction procedure. The organic supernatant was transferred to a new tube with 25 mg MgSO4 (≥99.99% pure, Sigma-Aldrich) and vortexed vigorously to remove water. After 10 min centrifugation at 1000 g, 80 µL of the final supernatant was spiked with instrumental internal standards (final concentration: 1 ng/mL) for analysis. Two 13C labeled chemicals [13C12]PCB-28 and [13C12]PBB-153 were used as volumetric internal standards added to the final extract, and nine 13C labeled chemicals (99% isotope enrichment for each) were spiked as recovery standards to estimate chemical recovery efficiency by XLE: [13C12]PCB-101, [13C12]PCB-153, [13C12]PCB-180, [13C12]PBDE-47, [13C12]PBDE-99, [13C6]anthracene, [13C10]mirex, [13C6]cis-permethrin, and [13C12]p,p’-DDE.

Sample Preparation:

Sampleprep ID:	SP001884
Sampleprep Summary:	Same as treatment

Combined analysis:

Analysis ID	AN002923
Analysis type	MS
Chromatography type	GC
Chromatography system	Thermo Trace 1310
Column	Agilent DB5-MS (15m x 0.25mm,0.25um)
MS Type	EI
MS instrument type	Orbitrap
MS instrument name	Thermo Q Exactive Orbitrap
Ion Mode	POSITIVE
Units

Chromatography:

Chromatography ID:	CH002165
Chromatography Summary:	Samples were analyzed with three injections using GC-HRMS with a Thermo Scientific Q Exactive GC hybrid quadrupole Orbitrap mass spectrometer with 2 µL per injection. A capillary DB-5MS column (15 m × 0.25 mm × 0.25 µm film thickness) was used with the following temperature program: hold 75 °C for 1 min, 25 °C/min to 180 °C, 6 °C/min to 250 °C, 20 °C/min to 350 °C and hold for 5 min. The flow rate of the helium carrier gas was 1 mL/min. Ion source and transfer line temperatures were 250°C and 280°C, respectively. Data were collected from 3 to 24.37 min with positive electron ionization (EI) mode (+70 eV), scanning from m/z 85.0000 to 850.0000 with a resolution of 60,000.
Instrument Name:	Thermo Trace 1310
Column Name:	Agilent DB5-MS (15m x 0.25mm,0.25um)
Chromatography Type:	GC

MS:

MS ID:	MS002715
Analysis ID:	AN002923
Instrument Name:	Thermo Q Exactive Orbitrap
Instrument Type:	Orbitrap
MS Type:	EI
MS Comments:	Data were collected from 3 to 24.37 min with positive electron ionization (EI) mode (+70 eV), scanning from m/z 85.0000 to 850.0000 with a resolution of 60,000. Raw data were examined by checking signal-to-noise ratio, peak shape and spectral information for surrogate and internal standards using a 5 ppm m/z tolerance and 30 s retention time window in xCalibur Qualbrowser software. Data extraction was performed by XCMS to generate about 40,000 chemical features identified by spectral m/z and retention time.
Ion Mode:	POSITIVE