#METABOLOMICS WORKBENCH edhummakupt_20150716_9661631_mwtab.txt DATATRACK_ID:344 STUDY_ID:ST000229 ANALYSIS_ID:AN000342 PROJECT_ID:PR000185 VERSION 1 CREATED_ON 2016-09-17 #PROJECT PR:PROJECT_TITLE Direct Analysis of Dried Blood Spots by Mass Spectrometry PR:PROJECT_TYPE Direct analysis methods, dried blood spots, MALDI, paper spray PR:PROJECT_SUMMARY The direct analysis methods of MALDI and paper spray ionization mass PR:PROJECT_SUMMARY were used to analyze dried blood spots without the need for punching out or PR:PROJECT_SUMMARY the samples. Ionization and instrument parameters were optimized, and a PR:PROJECT_SUMMARY method was developed for both techniques utilizing internal standards and a PR:PROJECT_SUMMARY isolation mass window. Additionally, the continuous addition of solvent to the PR:PROJECT_SUMMARY spray ionization setup was explored, as well as the use of a solvent gradient PR:PROJECT_SUMMARY potential sample clean-up. PR:INSTITUTE University of Florida PR:DEPARTMENT Chemistry PR:LABORATORY Chemistry Lab Building PR:LAST_NAME Yost PR:FIRST_NAME Richard PR:ADDRESS R3-226 Academic Research Building, Department of Biochemistry and Molecular PR:ADDRESS PO Box 100245, Gainesville, FL 32610-0245 PR:EMAIL ryost@chem.ufl.edu PR:PHONE 352-392-0515 PR:FUNDING_SOURCE SECIM U24 DK097209 #STUDY ST:STUDY_TITLE Analysis of Dried Blood Spots by Paper Spray Ionization - MS ST:STUDY_TYPE Analysis of Dried Blood Spots by Paper Spray Ionization - MS ST:STUDY_SUMMARY Concentrations of cocaine (6, 5,3,2,1.5,1,0.75,0.5,0.25,0.125, 0.062, and 0.031 ST:STUDY_SUMMARY were spiked into whole human blood for PS-MS analysis. A 10 uL volume of ST:STUDY_SUMMARY mixture was allowed to dry on Whatman Grade 2 filter paper. A 1ppm ST:STUDY_SUMMARY Cocaine-d3 was used as an internal standard. Parameters of the paper spray ST:STUDY_SUMMARY were optimized, including spray voltage, capillary temperature and solvent. The ST:STUDY_SUMMARY standard was added on top of the dried blood spot sample. Wide isolation tandem ST:STUDY_SUMMARY was used to generate a calibration curve. ST:INSTITUTE University of Florida ST:DEPARTMENT Chemistry ST:LABORATORY Chemistry Lab Building ST:LAST_NAME Dhummakupt ST:FIRST_NAME Elizabeth ST:ADDRESS R3-226 Academic Research Building, Department of Biochemistry and Molecular ST:ADDRESS PO Box 100245, Gainesville, FL 32610-0245 ST:EMAIL emuffly@ufl.edu ST:PHONE 352-392-0515 ST:NUM_GROUPS 11 ST:TOTAL_SUBJECTS 154 ST:STUDY_COMMENTS 11 concentrations were run as 7 samples/concentration for 2 days #SUBJECT SU:SUBJECT_TYPE Human SU:SUBJECT_SPECIES Homo sapiens SU:TAXONOMY_ID 9606 SU:GENDER Male #SUBJECT_SAMPLE_FACTORS: SUBJECT(optional)[tab]SAMPLE[tab]FACTORS(NAME:VALUE pairs separated by |)[tab]Additional sample data SUBJECT_SAMPLE_FACTORS - 1ppmCoc_1ppmCocd3_intensity_AVG Cocaine concentration (ppb):1000 Subject_type=Human whole blood; Day=Day 1 & day 2; Drug_spiked_in=Cocaine and Cocaine-d3 SUBJECT_SAMPLE_FACTORS - 125ppbCoc_1ppmCocd3_intensity_AVG Cocaine concentration (ppb):125 Subject_type=Human whole blood; Day=Day 1 & day 2; Drug_spiked_in=Cocaine and Cocaine-d3 SUBJECT_SAMPLE_FACTORS - 1.5ppmCoc_1ppmCocd3_intensity_AVG Cocaine concentration (ppb):1500 Subject_type=Human whole blood; Day=Day 1 & day 2; Drug_spiked_in=Cocaine and Cocaine-d3 SUBJECT_SAMPLE_FACTORS - 2ppmCoc_1ppmCocd3_intensity_AVG Cocaine concentration (ppb):2000 Subject_type=Human whole blood; Day=Day 1 & day 2; Drug_spiked_in=Cocaine and Cocaine-d3 SUBJECT_SAMPLE_FACTORS - 250ppbCoc_1ppmCocd3_intensity_AVG Cocaine concentration (ppb):250 Subject_type=Human whole blood; Day=Day 1 & day 2; Drug_spiked_in=Cocaine and Cocaine-d3 SUBJECT_SAMPLE_FACTORS - 3ppmCoc_1ppmCocd3_intensity_AVG Cocaine concentration (ppb):3000 Subject_type=Human whole blood; Day=Day 1 & day 2; Drug_spiked_in=Cocaine and Cocaine-d3 SUBJECT_SAMPLE_FACTORS - 31ppbCoc_1ppmCocd3_intensity_AVG Cocaine concentration (ppb):31 Subject_type=Human whole blood; Day=Day 1 & day 2; Drug_spiked_in=Cocaine and Cocaine-d3 SUBJECT_SAMPLE_FACTORS - 500ppbCoc_1ppmCocd3_intensity_AVG Cocaine concentration (ppb):500 Subject_type=Human whole blood; Day=Day 1 & day 2; Drug_spiked_in=Cocaine and Cocaine-d3 SUBJECT_SAMPLE_FACTORS - 5ppmCoc_1ppmCocd3_intensity_AVG Cocaine concentration (ppb):5000 Subject_type=Human whole blood; Day=Day 1 & day 2; Drug_spiked_in=Cocaine and Cocaine-d3 SUBJECT_SAMPLE_FACTORS - 6ppmCoc_1ppmCocd3_intensity_AVG Cocaine concentration (ppb):6000 Subject_type=Human whole blood; Day=Day 1 & day 2; Drug_spiked_in=Cocaine and Cocaine-d3 SUBJECT_SAMPLE_FACTORS - 62ppbCoc_1ppmCocd3_intensity_AVG Cocaine concentration (ppb):62 Subject_type=Human whole blood; Day=Day 1 & day 2; Drug_spiked_in=Cocaine and Cocaine-d3 SUBJECT_SAMPLE_FACTORS - 750ppbCoc_1ppmCocd3_intensity_AVG Cocaine concentration (ppb):750 Subject_type=Human whole blood; Day=Day 1 & day 2; Drug_spiked_in=Cocaine and Cocaine-d3 #COLLECTION CO:COLLECTION_SUMMARY - CO:SAMPLE_TYPE Blood CO:VOLUMEORAMOUNT_COLLECTED 20 mL CO:STORAGE_CONDITIONS Stored at 4 C CO:ADDITIVES NaEDTA #TREATMENT TR:TREATMENT_SUMMARY - TR:TREATMENT_PROTOCOL_COMMENTS Whole blood stored at 4 C; in liquid form, blood samples viable for 6 weeks #SAMPLEPREP SP:SAMPLEPREP_SUMMARY Addition of cocaine to blood samples SP:SAMPLE_SPIKING Unlabled cocaine was spiked into all samples. The deuterated cocaine was added SP:SAMPLE_SPIKING top of the dried spot. #CHROMATOGRAPHY CH:CHROMATOGRAPHY_TYPE - CH:INSTRUMENT_NAME - CH:COLUMN_NAME - #ANALYSIS AN:ANALYSIS_TYPE MS AN:LABORATORY_NAME Chemistry Lab Building AN:ACQUISITION_DATE 3/27/2015 & 4/2/2015 AN:ACQUISITION_PARAMETERS_FILE PSTune_Cocaine_Jan122015 AN:SOFTWARE_VERSION Xcalibur version 2.0 AN:OPERATOR_NAME Elizabeth Dhummakupt AN:DETECTOR_TYPE 3D Quadrupole Ion Trap AN:DATA_FORMAT .raw #MS MS:MS_COMMENTS - MS:INSTRUMENT_NAME Thermo Deca LCQ MS:INSTRUMENT_TYPE Ion trap MS:MS_TYPE Paper spray ionization MS:ION_MODE POSITIVE MS:CAPILLARY_TEMPERATURE 60 V MS:CAPILLARY_VOLTAGE 50 MS:COLLISION_ENERGY He MS:SOURCE_TEMPERATURE 4.0 kV MS:CDL_TEMPERATURE .raw MS:SAMPLE_DRIPPING m/z 80 - 500 MS:SKIMMER_VOLTAGE 15 V #MS_METABOLITE_DATA MS_METABOLITE_DATA:UNITS Avg Intensity MS_METABOLITE_DATA_START Samples 1ppmCoc_1ppmCocd3_intensity_AVG 125ppbCoc_1ppmCocd3_intensity_AVG 1.5ppmCoc_1ppmCocd3_intensity_AVG 2ppmCoc_1ppmCocd3_intensity_AVG 250ppbCoc_1ppmCocd3_intensity_AVG 3ppmCoc_1ppmCocd3_intensity_AVG 31ppbCoc_1ppmCocd3_intensity_AVG 500ppbCoc_1ppmCocd3_intensity_AVG 5ppmCoc_1ppmCocd3_intensity_AVG 6ppmCoc_1ppmCocd3_intensity_AVG 62ppbCoc_1ppmCocd3_intensity_AVG 750ppbCoc_1ppmCocd3_intensity_AVG Factors Cocaine concentration (ppb):1000 Cocaine concentration (ppb):125 Cocaine concentration (ppb):1500 Cocaine concentration (ppb):2000 Cocaine concentration (ppb):250 Cocaine concentration (ppb):3000 Cocaine concentration (ppb):31 Cocaine concentration (ppb):500 Cocaine concentration (ppb):5000 Cocaine concentration (ppb):6000 Cocaine concentration (ppb):62 Cocaine concentration (ppb):750 Cocaine 129228.5714 46982.7143 353205.7143 350207.1429 82786.4286 406452.1429 26964.4286 171614.2857 1004564.2860 702729.7143 30496.4286 210802.8571 Cocaine-d3 3457554.2860 1746742.8570 2069450.0000 4441500.0000 1288785.7140 1854971.4290 875057.1429 1323800.0000 2101714.2860 2458552.1430 1095700.0000 1424957.1430 MS_METABOLITE_DATA_END #METABOLITES METABOLITES_START metabolite_name moverz_quant ri ri_type pubchem_id inchi_key kegg_id other_id other_id_type Cocaine 182 UFLORIDA_FEATURE Cocaine-d3 185 UFLORIDA_FEATURE METABOLITES_END #END