#METABOLOMICS WORKBENCH tcavallo_20170105_095628 DATATRACK_ID:814 STUDY_ID:ST000535 ANALYSIS_ID:AN000814 PROJECT_ID:PR000394 VERSION 1 CREATED_ON January 24, 2017, 1:35 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 RTI International PR:DEPARTMENT Discovery-Sciences-Technology (DST) 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 I) 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 Discovery-Sciences-Technology (DST) 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, 400uL of the thawed urine sample were transferred to labeled SP:SAMPLEPREP_SUMMARY tubes on ice where they were mixed with 300uL of NMR Master Mix solution SP:SAMPLEPREP_SUMMARY containing Chenomx ISTD: DSS-d6 and D2O-Phosphate Buffer at 7.4 pH. Sample tubes SP:SAMPLEPREP_SUMMARY were vortexed for 2 min on a multi-tube vortexer and centrifuged at 16,000 rcf SP:SAMPLEPREP_SUMMARY for 5 min. A 600uL of each sample supernatant was transferred into a pre-labeled SP:SAMPLEPREP_SUMMARY 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:SPECTROMETER_FREQUENCY 700 MHz NM:NMR_PROBE 5mm ATMA Cryoprobe NM:NMR_SOLVENT D NM:NMR_TUBE_SIZE 5 NM:SHIMMING_METHOD Topshim NM:PULSE_SEQUENCE noesypr1d NM:WATER_SUPPRESSION yes NM:PULSE_WIDTH 13.0s NM:POWER_LEVEL 25.119W NM:RECEIVER_GAIN 4.5 NM:OFFSET_FREQUENCY 3296 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 0.5Hz 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-Methylnicotinamide 23.4 31.4 31.9 29 23.8 27.8 2-Aminoadipate 254.7 257 255.3 262.5 260.5 269.2 2-Furoylglycine 79.7 76.1 69.8 81.3 76.7 78.6 2-Hydroxyisobutyrate 30.3 30.7 30.1 31.9 30.2 33.4 3,5-Dibromotyrosine 302.9 308.5 311.8 311.5 340.6 316.7 3-Aminoisobutyrate 120.2 109.1 116.9 113.1 117.8 122.5 3-Hydroxyisovalerate 47.9 44.4 44.5 45.9 46.2 48 3-Indoxylsulfate 176 173 164 163.1 177.7 180.9 3-Methyl-2-oxovalerate 43.5 69.7 80.4 85.3 74.6 79.6 5-Hydroxytryptophan 84.6 77 109.5 119 119.4 118.7 Acetate 11260.5 11188.6 11300.4 11322.5 11329.4 11301.5 Alanine 154.2 157.7 155.2 162.5 161.5 160.2 Benzoate 37.3 46.5 49.5 42.7 42.8 46.7 Betaine 175.6 169.1 146.6 167.3 167.3 177 Citrate 1244.6 1304.1 1297.4 1289.4 1280.7 1294 Creatine 747.9 734.4 721 737.3 722.7 721.5 Creatine phosphate 450.1 440 440.7 459.1 461.7 468.3 Creatinine 4004.8 4181.8 4067 4078.5 4109.1 4076 Dimethylamine 88.8 100.5 92.9 94.8 91.4 100.7 Ethanol 907.9 929.1 909.8 948 929 934.8 Formate 352.2 371.1 365.7 374.3 363.5 366.2 Gluconate 1181.7 1255 1170.3 1265.5 1261.3 1249.9 Glucose 4698.2 5020.6 5047.3 4425.3 4943.9 4922.9 Glycerol 234.7 162.8 183.6 152.1 154.9 189.6 Glycine 817.5 842.1 830.9 860.4 835.8 838.6 Glycolate 400.3 559 557.2 525.4 526.2 535.2 Hippurate 947.9 968.9 959.4 971.9 946.3 1038.7 Histamine 278.6 223.2 328.6 348.9 315.7 305.5 Histidine 326.8 316.8 294.3 296.6 291.2 299.1 Isoleucine 25.1 15.7 21.2 24.2 23.7 24.9 Lactate 407.4 414.4 417.2 423.1 428.4 408.4 Leucine 24.4 21.7 23.2 25 25.6 28 Lysine 189 168.5 181.9 180.8 193.3 190.2 Methanol 1936 117.1 118.8 119.1 117 116.4 Methylmalonate 189.6 191.6 189.6 189.7 188.7 188.8 N,N-Dimethylformamide 46.8 66.5 66.5 67 64.5 67.2 N,N-Dimethylglycine 25.3 24.6 24.5 25.5 25.6 25.5 N-Acetylaspartate 81.7 81.3 82.4 82.7 82.2 82.1 O-Acetylcholine 58 48.6 47.8 48.6 48.3 47.5 Phenylalanine 325 339.6 336.6 302.2 326.3 334.6 Propionate 152.6 160.8 180.5 165.5 161.8 165.4 Propylene glycol 105.5 107.7 108.5 113.6 105.5 109.5 Pyruvate 124.4 152 146.3 146 151.2 129.1 Sarcosine 179.8 171.2 179.2 186.6 184.5 192.6 Succinate 117.2 120.8 118.5 122.9 121 133.9 Taurine 522.5 570.6 545.5 566.9 580 582 Threonate 802.3 824.1 707 669.8 637.9 696.8 Trigonelline 102.7 105.6 106.8 106.5 108 103.6 Trimethylamine 40.5 42.1 40.6 42 41.9 42.2 Trimethylamine N-oxide 207.2 225.3 235.9 225.1 223.5 217.7 Tryptophan 173.5 177.5 187.1 183.7 190.2 182.6 Tyrosine 57.5 63.3 63.2 63.8 59.8 62.7 Urea 29797.8 30184.6 30221.6 33295.2 30582.8 33942.5 Valine 24.6 25.2 25.5 26.2 20.6 25.4 Valproate 39.1 28.3 22.2 27.8 27.5 31.3 cis-Aconitate 37.4 27.5 26.4 35.6 42.7 22.2 sn-Glycero-3-phosphocholine 32.9 31.1 29.5 75 34.3 34 trans-Aconitate 92 91 90.3 95.3 94.1 94.2 π-Methylhistidine 198.7 265.5 206.9 183.8 178.1 202.4 τ-Methylhistidine 149.9 152.8 152.8 158.8 157.9 151 NMR_METABOLITE_DATA_END #METABOLITES METABOLITES_START metabolite_name retention index quantified m/z PubChem ID KEGG ID 1-Methylnicotinamide 2-Aminoadipate 2-Furoylglycine 2-Hydroxyisobutyrate 3,5-Dibromotyrosine 3-Aminoisobutyrate 3-Hydroxyisovalerate 3-Indoxylsulfate 3-Methyl-2-oxovalerate 5-Hydroxytryptophan Acetate Alanine Benzoate Betaine Citrate Creatine Creatine phosphate Creatinine Dimethylamine Ethanol Formate Gluconate Glucose Glycerol Glycine Glycolate Hippurate Histamine Histidine Isoleucine Lactate Leucine Lysine Methanol Methylmalonate N,N-Dimethylformamide N,N-Dimethylglycine N-Acetylaspartate O-Acetylcholine Phenylalanine Propionate Propylene glycol Pyruvate Sarcosine Succinate Taurine Threonate Trigonelline Trimethylamine Trimethylamine N-oxide Tryptophan Tyrosine Urea Valine Valproate cis-Aconitate sn-Glycero-3-phosphocholine trans-Aconitate π-Methylhistidine τ-Methylhistidine METABOLITES_END #END