#METABOLOMICS WORKBENCH mwortham_20180427_120539 DATATRACK_ID:1390 STUDY_ID:ST000964 ANALYSIS_ID:AN001578 PROJECT_ID:PR000662 VERSION 1 CREATED_ON April 30, 2018, 12:09 pm #PROJECT PR:PROJECT_TITLE Integrated in vivo quantitative proteomics and nutrient tracing reveals PR:PROJECT_TITLE age-related metabolic rewiring of pancreatic beta cell function PR:PROJECT_SUMMARY Aging is associated with fundamental changes in pancreatic β-cell physiology; PR:PROJECT_SUMMARY yet, the mechanisms that drive these age-related changes are poorly understood. PR:PROJECT_SUMMARY Here, we performed comprehensive in vivo quantitative proteomic profiling of PR:PROJECT_SUMMARY pancreatic islets from adolescent and old mice. Nutrient tracing and targeted PR:PROJECT_SUMMARY metabolomics demonstrated accelerated accumulation of glucose-derived PR:PROJECT_SUMMARY metabolites and coupling factors in aged islets, indicating that age-related PR:PROJECT_SUMMARY changes in glucose metabolism contribute to improved glucose-stimulated insulin PR:PROJECT_SUMMARY secretion with age. Together, our study provides the first in-depth PR:PROJECT_SUMMARY characterization of age-related changes in the islet proteome and establishes PR:PROJECT_SUMMARY metabolic rewiring as an important mechanism for age-associated changes in PR:PROJECT_SUMMARY β-cell function. PR:INSTITUTE University of California, San Diego PR:LAST_NAME Wortham PR:FIRST_NAME Matthew PR:ADDRESS 2880 Torrey Pines Scenic Drive, Sanford Consortium for Regenerative Medicine, PR:ADDRESS Room 3102, La Jolla, California, 92037, USA PR:EMAIL mwortham@ucsd.edu PR:PHONE 8582460588 #STUDY ST:STUDY_TITLE U13C Glucose Tracing of Young and Old Pancreatic Islets ST:STUDY_SUMMARY Pancreatic islets from young and old mice were traced with either 2.8mM or ST:STUDY_SUMMARY 16.8mM U13C glucose to determine the effect of age upon glucose metabolism in ST:STUDY_SUMMARY basal and stimulated states. ST:INSTITUTE University of California, San Diego ST:LAST_NAME Wortham ST:FIRST_NAME Matthew ST:ADDRESS 2880 Torrey Pines Scenic Drive, Sanford Consortium for Regenerative Medicine, ST:ADDRESS Room 3102 ST:EMAIL mwortham@ucsd.edu ST:PHONE 8582460588 #SUBJECT SU:SUBJECT_TYPE Mammal SU:SUBJECT_SPECIES Mus musculus SU:TAXONOMY_ID 10090 SU:GENOTYPE_STRAIN C57BL/6N SU:AGE_OR_AGE_RANGE 4 weeks old (young) or 10-15 months old (old) SU:GENDER Male and female SU:ANIMAL_ANIMAL_SUPPLIER Charles River Labs SU:ANIMAL_FEED standard chow diet (PicoLab Rodent Diet 20 pellets, #5053 #SUBJECT_SAMPLE_FACTORS: SUBJECT(optional)[tab]SAMPLE[tab]FACTORS(NAME:VALUE pairs separated by |)[tab]Additional sample data SUBJECT_SAMPLE_FACTORS - 10_25_2016_islet_YA_1 Age:Young (4 weeks) | Treatment:2.8mM Glucose (60 min) SUBJECT_SAMPLE_FACTORS - 10_25_2016_islet_YB_2 Age:Young (4 weeks) | Treatment:2.8mM Glucose (60 min) SUBJECT_SAMPLE_FACTORS - 10_25_2016_islet_YC_3 Age:Young (4 weeks) | Treatment:2.8mM Glucose (60 min) SUBJECT_SAMPLE_FACTORS - 10_25_2016_islet_YD_4 Age:Young (4 weeks) | Treatment:2.8mM Glucose (60 min) SUBJECT_SAMPLE_FACTORS - 10_25_2016_islet_YE_5 Age:Young (4 weeks) | Treatment:2.8mM Glucose (60 min) SUBJECT_SAMPLE_FACTORS - 10_25_2016_islet_YHA_6 Age:Young (4 weeks) | Treatment:16.8mM Glucose (60 min) SUBJECT_SAMPLE_FACTORS - 10_25_2016_islet_YHB_7 Age:Young (4 weeks) | Treatment:16.8mM Glucose (60 min) SUBJECT_SAMPLE_FACTORS - 10_25_2016_islet_YHC_8 Age:Young (4 weeks) | Treatment:16.8mM Glucose (60 min) SUBJECT_SAMPLE_FACTORS - 10_25_2016_islet_YHD_9 Age:Young (4 weeks) | Treatment:16.8mM Glucose (60 min) SUBJECT_SAMPLE_FACTORS - 10_25_2016_islet_YHE_10 Age:Young (4 weeks) | Treatment:16.8mM Glucose (60 min) SUBJECT_SAMPLE_FACTORS - 10_25_2016_islet_YHF_11 Age:Young (4 weeks) | Treatment:16.8mM Glucose (60 min) SUBJECT_SAMPLE_FACTORS - 10_25_2016_islet_OA_12 Age:Old (10-15 months) | Treatment:2.8mM Glucose (60 min) SUBJECT_SAMPLE_FACTORS - 10_25_2016_islet_OB_13 Age:Old (10-15 months) | Treatment:2.8mM Glucose (60 min) SUBJECT_SAMPLE_FACTORS - 10_25_2016_islet_OC_14 Age:Old (10-15 months) | Treatment:2.8mM Glucose (60 min) SUBJECT_SAMPLE_FACTORS - 10_25_2016_islet_OD_15 Age:Old (10-15 months) | Treatment:2.8mM Glucose (60 min) SUBJECT_SAMPLE_FACTORS - 10_25_2016_islet_OHA_16 Age:Old (10-15 months) | Treatment:16.8mM Glucose (60 min) SUBJECT_SAMPLE_FACTORS - 10_25_2016_islet_OHB_17 Age:Old (10-15 months) | Treatment:16.8mM Glucose (60 min) SUBJECT_SAMPLE_FACTORS - 10_25_2016_islet_OHC_18 Age:Old (10-15 months) | Treatment:16.8mM Glucose (60 min) SUBJECT_SAMPLE_FACTORS - 10_25_2016_islet_OHD_19 Age:Old (10-15 months) | Treatment:16.8mM Glucose (60 min) SUBJECT_SAMPLE_FACTORS - 10_25_2016_islet_OHE_20 Age:Old (10-15 months) | Treatment:16.8mM Glucose (60 min) #COLLECTION CO:COLLECTION_SUMMARY Pancreata were digested using Liberase TL, and islets were purified using a CO:COLLECTION_SUMMARY Histopaque gradient followed by hand-picking under a dissecting microscope. CO:COLLECTION_SUMMARY Islets were allowed to recover overnight in RPMI 1640 media supplemented with 8 CO:COLLECTION_SUMMARY mM glucose, 10% FBS, 2 mM L-glutamine, 100 U/mL Pen/Strep, 1 mM sodium pyruvate, CO:COLLECTION_SUMMARY 10 mM HEPES, and 0.25 mg/mL amphoterecin B. CO:COLLECTION_PROTOCOL_FILENAME Methods.pdf CO:SAMPLE_TYPE Pancreatic Islets #TREATMENT TR:TREATMENT_SUMMARY Islets were starved for 1 hour in KRBH supplemented with 2.8 mM glucose as for TR:TREATMENT_SUMMARY GSIS assays. Islets were then transferred to petri dishes containing TR:TREATMENT_SUMMARY U-13C-labeled glucose as indicated and immediately seeded into wells of TR:TREATMENT_SUMMARY non-treated 12-well plates at a density of 100 size-matched islets per replicate TR:TREATMENT_SUMMARY in a final volume of 500 μl KRBH containing basal (2.8 mM) or stimulatory (16.8 TR:TREATMENT_SUMMARY mM) concentrations of labeled glucose. Tracing was performed for the indicated TR:TREATMENT_SUMMARY durations at 37oC with 5% CO2. Following the trace, islets were rapidly chilled TR:TREATMENT_SUMMARY by swirling plate to resuspend islets then transferring entire contents of each TR:TREATMENT_SUMMARY well to an Eppendorf tube on ice. Islets were then pelleted by centrifugation at TR:TREATMENT_SUMMARY 500 x g for 2 min at 4oC, washed in 1 mL of ice cold 0.9% NaCl, centrifuged as TR:TREATMENT_SUMMARY before, then pellets were frozen in a dry ice/ethanol bath and stored at -80oC. #SAMPLEPREP SP:SAMPLEPREP_SUMMARY Metabolites were extracted from pellets using a bligh and dyer-based SP:SAMPLEPREP_SUMMARY methanol/chloroform/water extraction with inclusion of norvaline as a polar SP:SAMPLEPREP_SUMMARY internal standard. Briefly, 250 μl MeOH, 250 μl CHCL3, 100 μl water SP:SAMPLEPREP_SUMMARY containing norvaline were added to pellets. This was vortexed for 10 minutes SP:SAMPLEPREP_SUMMARY followed by centrifugation at 10,000 g for 5 minutes at 4°C. The upper phase SP:SAMPLEPREP_SUMMARY was separated and dried under vacuum at 4°C until dry. Polar metabolites were SP:SAMPLEPREP_SUMMARY derivatized in 2% (w/v) methoxyamine hydrochloride in pyridine and incubated at SP:SAMPLEPREP_SUMMARY 45°C for 60 minutes. Samples were then silylated with SP:SAMPLEPREP_SUMMARY N-tertbutyldimethylsilyl-N-methyltrifluoroacetamide (MtBSTFA) with 1% SP:SAMPLEPREP_SUMMARY tert-butyldimethylchlorosilane (tBDMCS) at 45°C for 30 minutes. Polar SP:SAMPLEPREP_SUMMARY derivatives were analyzed by GC-MS using a DB-35MS column (30m x 0.25 mm i.d. x SP:SAMPLEPREP_SUMMARY 0.25 μm) installed in an Agilent 7890B gas chromatograph (GC) interfaced with SP:SAMPLEPREP_SUMMARY an Agilent 5977A mass spectrometer (MS) with an XTR EI source using the SP:SAMPLEPREP_SUMMARY following temperature program: 100 °C initial, increase by 3.5 °C/min to 255 SP:SAMPLEPREP_SUMMARY °C, increase by 15 °C/min to 320 °C and hold for 3 min. #CHROMATOGRAPHY CH:CHROMATOGRAPHY_SUMMARY Polar derivatives were analyzed by GC-MS using a DB-35MS column (30m x 0.25 mm CH:CHROMATOGRAPHY_SUMMARY i.d. x 0.25 μm) installed in an Agilent 7890B gas chromatograph (GC) interfaced CH:CHROMATOGRAPHY_SUMMARY with an Agilent 5977A mass spectrometer (MS) with an XTR EI source using the CH:CHROMATOGRAPHY_SUMMARY following temperature program: 100 °C initial, increase by 3.5 °C/min to 255 CH:CHROMATOGRAPHY_SUMMARY °C, increase by 15 °C/min to 320 °C and hold for 3 min. CH:CHROMATOGRAPHY_TYPE GC CH:INSTRUMENT_NAME Agilent 7890B CH:COLUMN_NAME Agilent DB5-MS (15m × 0.25mm) #ANALYSIS AN:ANALYSIS_TYPE MS #MS MS:MS_COMMENTS - MS:INSTRUMENT_NAME Agilent 5977A MS:INSTRUMENT_TYPE Single quadrupole MS:MS_TYPE EI MS:ION_MODE POSITIVE #MS_METABOLITE_DATA MS_METABOLITE_DATA:UNITS Total ion counts MS_METABOLITE_DATA_START Samples 10_25_2016_islet_YA_1 10_25_2016_islet_YB_2 10_25_2016_islet_YC_3 10_25_2016_islet_YD_4 10_25_2016_islet_YE_5 10_25_2016_islet_YHA_6 10_25_2016_islet_YHB_7 10_25_2016_islet_YHC_8 10_25_2016_islet_YHD_9 10_25_2016_islet_YHE_10 10_25_2016_islet_YHF_11 10_25_2016_islet_OA_12 10_25_2016_islet_OB_13 10_25_2016_islet_OC_14 10_25_2016_islet_OD_15 10_25_2016_islet_OHA_16 10_25_2016_islet_OHB_17 10_25_2016_islet_OHC_18 10_25_2016_islet_OHD_19 10_25_2016_islet_OHE_20 10_25_2016_islet_YHE_10 10_25_2016_islet_YHF_11 Factors Age:Young (4 weeks) | Treatment:2.8mM Glucose (60 min) Age:Young (4 weeks) | Treatment:2.8mM Glucose (60 min) Age:Young (4 weeks) | Treatment:2.8mM Glucose (60 min) Age:Young (4 weeks) | Treatment:2.8mM Glucose (60 min) Age:Young (4 weeks) | Treatment:2.8mM Glucose (60 min) Age:Young (4 weeks) | Treatment:16.8mM Glucose (60 min) Age:Young (4 weeks) | Treatment:16.8mM Glucose (60 min) Age:Young (4 weeks) | Treatment:16.8mM Glucose (60 min) Age:Young (4 weeks) | Treatment:16.8mM Glucose (60 min) Age:Young (4 weeks) | Treatment:16.8mM Glucose (60 min) Age:Young (4 weeks) | Treatment:16.8mM Glucose (60 min) Age:Old (10-15 months) | Treatment:2.8mM Glucose (60 min) Age:Old (10-15 months) | Treatment:2.8mM Glucose (60 min) Age:Old (10-15 months) | Treatment:2.8mM Glucose (60 min) Age:Old (10-15 months) | Treatment:2.8mM Glucose (60 min) Age:Old (10-15 months) | Treatment:16.8mM Glucose (60 min) Age:Old (10-15 months) | Treatment:16.8mM Glucose (60 min) Age:Old (10-15 months) | Treatment:16.8mM Glucose (60 min) Age:Old (10-15 months) | Treatment:16.8mM Glucose (60 min) Age:Old (10-15 months) | Treatment:16.8mM Glucose (60 min) Age:Young (4 weeks) | Treatment:16.8mM Glucose (60 min) Age:Young (4 weeks) | Treatment:16.8mM Glucose (60 min) Pyruvic acid 127872 112204 144461 100184 127227 171618 125279 238191 147351 137885 273982 125525 125669 120114 138049 143772 263368 160353 165116 257911 137885 273982 Alanine 149331 176595 170978 92567 158648 225310 199434 297371 263588 216610 270899 129018 124160 157740 165844 166813 331445 188564 322864 276523 216610 270899 Glycine 1039556 1144609 1070311 626542 962526 906185 846861 1137254 1129803 906314 984481 1111236 933364 1404425 1202776 800997 1461625 965475 1538193 1330172 906314 984481 Norvaline 4871730 5862696 5271742 3623930 4816000 4481891 4621497 5607100 4805219 4890895 4986328 5060059 5192042 6270470 5029168 4209004 5193592 4220621 4848393 4889503 4890895 4986328 Fumaric acid 76644 89683 95824 70225 65259 204151 218227 164364 235746 223585 186575 88000 104780 63468 90678 268930 333936 222095 450449 313598 223585 186575 Malic acid 34985 47351 41842 145211 43924 409443 378689 597403 414248 430598 436624 50596 50206 56805 49845 443331 753516 488383 891031 754076 430598 436624 Aspartic acid 1258378 1631993 1709001 744237 1441617 1017961 949464 1745570 1419668 998841 1405252 991603 691648 1059798 1069099 558917 1480591 685144 1369715 905781 998841 1405252 Glutamic acid 1551470 2384163 2342152 1045410 2031316 1613981 1502895 2538828 2054041 1631004 2000736 1733091 1220167 1825296 1808941 828959 2399020 1142550 2499607 1707531 1631004 2000736 Citric acid 227796 403797 338957 133857 216051 515702 498069 761536 629775 495454 404636 146875 112900 137748 158354 294254 664080 361940 731834 528354 495454 404636 MS_METABOLITE_DATA_END #METABOLITES METABOLITES_START metabolite_name m/z Pyruvic acid 174 Alanine 260 Glycine 246 Norvaline 260 Fumaric acid 287 Malic acid 419 Aspartic acid 418 Glutamic acid 432 Citric acid 459 METABOLITES_END #END