#METABOLOMICS WORKBENCH tcavallo_20170119_090307 DATATRACK_ID:824 STUDY_ID:ST000538 ANALYSIS_ID:AN000817 PROJECT_ID:PR000394 VERSION 1 CREATED_ON January 24, 2017, 1:52 pm #PROJECT PR:PROJECT_TITLE CHEAR Urine Reference Material Proficiency Test NMR PR:PROJECT_TYPE CHEAR-UT-1 PR:PROJECT_SUMMARY CHEAR Reference Material Urine was provided by Emory University. The material PR:PROJECT_SUMMARY was prepared and analyzed using the NMR metabolomics workflow of the Eastern PR:PROJECT_SUMMARY Regional Metabolomics Resource Core. Data of six samples were acquired of the PR:PROJECT_SUMMARY sample reference material prepared in replicate. PR:INSTITUTE NIEHS PR:DEPARTMENT CHEAR - Children's Health Exposure Analysis Resource PR:LABORATORY RTI CHEAR Analytical Hub - Untargeted Analysis Resource Core PR:LAST_NAME Fennell PR:FIRST_NAME Timothy PR:ADDRESS 3040 E Cornwallis Road, Research Triangle Park, NC 27709 PR:EMAIL fennell@rti.org PR:PHONE 919-485-2781 #STUDY ST:STUDY_TITLE CHEAR Urine Reference Material Proficiency Test NMR (Part II) ST:STUDY_TYPE Metabolomics ST:STUDY_SUMMARY CHEAR Reference Material Urine was provided by Emory University. The material ST:STUDY_SUMMARY was prepared and analyzed using the NMR metabolomics workflow of the Eastern ST:STUDY_SUMMARY Regional Metabolomics Resource Core. Data of six samples were acquired of the ST:STUDY_SUMMARY sample reference material prepared in replicate. ST:INSTITUTE RTI International ST:DEPARTMENT Analytical Chemistry & Pharmaceuticals ST:LABORATORY RTI CHEAR Analytical Hub - Untargeted Analysis Resource Core ST:LAST_NAME Fennell ST:FIRST_NAME Timothy ST:ADDRESS 3040 E Cornwallis Road, Research Triangle Park, NC 27709 ST:EMAIL fennell@rti.org ST:PHONE 919-485-2781 #SUBJECT SU:SUBJECT_TYPE Human SU:SUBJECT_SPECIES Homo sapiens SU:TAXONOMY_ID 9606 #SUBJECT_SAMPLE_FACTORS: SUBJECT(optional)[tab]SAMPLE[tab]FACTORS(NAME:VALUE pairs separated by |)[tab]Additional sample data SUBJECT_SAMPLE_FACTORS - U_1 Sample Type:Replicate CHEAR ID=CHE000066; Aliquot ID=210 SUBJECT_SAMPLE_FACTORS - U_2 Sample Type:Replicate CHEAR ID=CHE000066; Aliquot ID=220 SUBJECT_SAMPLE_FACTORS - U_3 Sample Type:Replicate CHEAR ID=CHE000066; Aliquot ID=230 SUBJECT_SAMPLE_FACTORS - U_4 Sample Type:Replicate CHEAR ID=CHE000066; Aliquot ID=240 SUBJECT_SAMPLE_FACTORS - U_5 Sample Type:Replicate CHEAR ID=CHE000066; Aliquot ID=250 SUBJECT_SAMPLE_FACTORS - U_6 Sample Type:Replicate CHEAR ID=CHE000066; Aliquot ID=260 #COLLECTION CO:COLLECTION_SUMMARY CHEAR Reference Material Urine was provided by Emory University. #TREATMENT TR:TREATMENT_SUMMARY None #SAMPLEPREP SP:SAMPLEPREP_SUMMARY A total of 6 CHEAR Urine Reference Material aliquots were thawed on ice for SP:SAMPLEPREP_SUMMARY sample preparation, 400 L of the thawed urine sample were transferred to SP:SAMPLEPREP_SUMMARY labeled tubes on ice where they were mixed with 300 L of NMR Master Mix SP:SAMPLEPREP_SUMMARY solution containing Chenomx ISTD: DSS-d6 and D2O-Phosphate Buffer at 7.4 pH. SP:SAMPLEPREP_SUMMARY Sample tubes were vortexed for 2 min on a multi-tube vortexer and centrifuged at SP:SAMPLEPREP_SUMMARY 16,000 rcf for 5 min. A 600 L of each sample supernatant was transferred into SP:SAMPLEPREP_SUMMARY a pre-labeled 5mm 4" NMR tubes for data acquisition on a 700 MHz spectrometer. #CHROMATOGRAPHY CH:CHROMATOGRAPHY_TYPE - CH:INSTRUMENT_NAME - CH:COLUMN_NAME - #ANALYSIS AN:ANALYSIS_TYPE NMR #NMR NM:INSTRUMENT_NAME Bruker NM:INSTRUMENT_TYPE FT-NMR NM:NMR_EXPERIMENT_TYPE 1D-1H NM:FIELD_FREQUENCY_LOCK Deuterium NM:STANDARD_CONCENTRATION 0.5mM NM:SPECTROMETER_FREQUENCY 700 MHz NM:NMR_PROBE 5mm ATMA Cryoprobe NM:NMR_SOLVENT D2O NM:NMR_TUBE_SIZE 5mm NM:SHIMMING_METHOD top shim NM:PULSE_SEQUENCE noesypr1d NM:WATER_SUPPRESSION yes NM:PULSE_WIDTH 13.0us NM:POWER_LEVEL 25.119 W NM:RECEIVER_GAIN 4.5 NM:OFFSET_FREQUENCY 3296 Hz NM:CHEMICAL_SHIFT_REF_CPD DSS NM:TEMPERATURE 300K NM:NUMBER_OF_SCANS 64 NM:DUMMY_SCANS 4 NM:ACQUISITION_TIME 3.9s NM:RELAXATION_DELAY 2s NM:SPECTRAL_WIDTH 12.02ppm NM:NUM_DATA_POINTS_ACQUIRED 65536 NM:REAL_DATA_POINTS 32768 NM:LINE_BROADENING 0.5 Hz NM:ZERO_FILLING yes NM:APODIZATION Lorentzian NM:BASELINE_CORRECTION_METHOD Polynomial NM:CHEMICAL_SHIFT_REF_STD DSS-d6 #NMR_METABOLITE_DATA NMR_METABOLITE_DATA:UNITS uM NMR_METABOLITE_DATA_START Samples U_1 U_2 U_3 U_4 U_5 U_6 Factors Sample Type:Replicate Sample Type:Replicate Sample Type:Replicate Sample Type:Replicate Sample Type:Replicate Sample Type:Replicate 1,6-Anhydro-β-D-glucose 115.9 121.7 129.8 122.7 118.8 121 1-Methylnicotinamide 25.5 26.6 28.8 30.5 31.4 28.9 2-Aminoadipate 189.9 193.4 185.9 214.2 168.2 185.8 2-Furoylglycine 81.9 65 69.6 70.8 59.3 70.9 2-Hydroxy-3-methylvalerate 33.9 25.9 26.5 22.3 21.4 22.8 2-Hydroxybutyrate 46.8 28.5 32.5 23.9 38.3 37.2 2-Hydroxyisobutyrate 24.7 25.5 24.6 26.4 25.2 23.9 2-Methylglutarate 39.8 41.3 31.8 35.3 30.3 38.3 2-Oxobutyrate 168.8 168.5 173.2 163.5 173.5 177.2 3-Aminoisobutyrate 82.6 62.4 83.4 73.3 73.6 76.7 3-Hydroxyisovalerate 38.8 38.7 38 36.6 34.5 33.8 3-Indoxylsulfate 162.2 132.6 156.3 130.3 141 152.4 Acetate 11268.6 11244.9 11304.7 11248.4 11330.7 11298.8 Acetoacetate 31.2 37.2 43.6 33.6 31 32.7 Acetoin 42.8 38.8 43 45.5 41.5 45.5 Alanine 138.2 145 140.4 142.7 143.7 141.9 Allantoin 82.9 73.1 84.4 65.8 79.7 66.8 Citrate 1100.9 1145.5 1015.8 1088.3 1026.6 1059.5 Creatine 703.9 732.6 712.6 731.5 717.9 715.9 Creatinine 4096.8 4203.1 4069.2 4080.9 4112 4077.8 Dimethylamine 196 205.2 200.7 206.5 201.2 202.2 Ethanol 853.8 934.3 911.1 948.4 930 934.5 Formate 352.3 374.5 365.3 374 363.7 364.3 Gluconate 1044.6 1146.5 1099.2 1181.5 1161.6 1117 Glucose 4313.5 4336.6 4156 4407.2 4197.2 4299.3 Glycine 819.8 849.1 834.9 864.7 839.1 841.7 Glycolate 305.8 265.1 261.3 268.9 270.5 269.1 Hippurate 889.4 965.1 1001.1 1008.2 877.7 995.8 Hypoxanthine 21.1 18.1 25.8 18.4 19.3 19.2 Lactate 401.1 407.5 420 421.4 405.6 404.5 Methanol 1934.3 581 666.5 570.5 659.2 600.9 Methylmalonate 109.7 81.8 100.6 113.5 74.2 87.5 N,N-Dimethylglycine 14.1 13.2 12.7 13.2 13.1 13.1 N-Acetyltyrosine 74.3 64.7 77.7 83.7 78.1 64.4 N-Phenylacetylglycine 311 281.8 261.1 286.7 306.1 332.8 Phenylalanine 45.3 71.9 87.6 70 66.4 68 Propylene glycol 66 59 82.1 65.4 75.7 70.8 Pyruvate 124.5 152.7 146.5 146.2 151.1 129.2 Succinate 117.2 121.2 118.6 122.9 121 120.6 Sucrose 55.7 54 51.2 51.3 46.8 46.3 Threonine 13.3 16.7 12.2 15.6 13.7 11.2 Trigonelline 97.4 98.8 101.4 99.3 101 96.4 Trimethylamine 9.6 11.2 10 11.2 9.7 11.1 Trimethylamine N-oxide 345 354.1 365.2 367.9 343.1 359.8 Tryptophan 51 42.6 45.6 48.2 48.6 45.3 Tyrosine 42.1 45.5 44.4 49.9 36.3 40.2 Urea 26482.8 26953.1 27164.4 29344 27389.3 30064.6 Xanthine 40.5 46.2 50.3 39.9 51 46.7 cis-Aconitate 158.5 145.2 150.4 174 174.2 156.6 trans-Aconitate 91.7 91.4 90.3 95.2 83.7 93.7 π-Methylhistidine 134.7 145.4 141.8 159.5 137.7 143.7 NMR_METABOLITE_DATA_END #METABOLITES METABOLITES_START metabolite_name retention index quantified m/z PubChem ID KEGG ID 1,6-Anhydro-β-D-glucose 1-Methylnicotinamide 2-Aminoadipate 2-Furoylglycine 2-Hydroxy-3-methylvalerate 2-Hydroxybutyrate 2-Hydroxyisobutyrate 2-Methylglutarate 2-Oxobutyrate 3-Aminoisobutyrate 3-Hydroxyisovalerate 3-Indoxylsulfate Acetate Acetoacetate Acetoin Alanine Allantoin Citrate Creatine Creatinine Dimethylamine Ethanol Formate Gluconate Glucose Glycine Glycolate Hippurate Hypoxanthine Lactate Methanol Methylmalonate N,N-Dimethylglycine N-Acetyltyrosine N-Phenylacetylglycine Phenylalanine Propylene glycol Pyruvate Succinate Sucrose Threonine Trigonelline Trimethylamine Trimethylamine N-oxide Tryptophan Tyrosine Urea Xanthine cis-Aconitate trans-Aconitate π-Methylhistidine METABOLITES_END #END