#METABOLOMICS WORKBENCH nozomu_kono_20211017_174345 DATATRACK_ID:2892 STUDY_ID:ST001951 ANALYSIS_ID:AN003176 PROJECT_ID:PR001238 VERSION 1 CREATED_ON October 23, 2021, 3:27 pm #PROJECT PR:PROJECT_TITLE Analysis of ω-3 fatty acids and their derivatives in lungs from hypoxia-induced PR:PROJECT_TITLE pulmonary hypertension (PH) mice. PR:PROJECT_SUMMARY Pulmonary arterial hypertension (PAH) is a rare, fatal disease that causes PR:PROJECT_SUMMARY idiopathic pulmonary artery stenosis, which leads to increased pulmonary artery PR:PROJECT_SUMMARY pressure and this chronic pressure-overload eventually results in right heart PR:PROJECT_SUMMARY failure and death. Although the available therapies for PH have notably improved PR:PROJECT_SUMMARY the survival of patients with PAH, there is still a significant portion of PR:PROJECT_SUMMARY patients who do not achieve the expected efficacy. Here, in order to identify PR:PROJECT_SUMMARY bioactive lipids which are protective against pulmonary hypertension (PH), we PR:PROJECT_SUMMARY performed comprehensive lipidomic analysis of lung samples from hypoxia-induced PR:PROJECT_SUMMARY PH mice. PR:INSTITUTE University of Tokyo PR:LAST_NAME Kono PR:FIRST_NAME Nozomu PR:ADDRESS 7-3-1, Hongo, Bunkyo-ku, Tokyo 113-0033, Japan PR:EMAIL nozomu@mol.f.u-tokyo.ac.jp PR:PHONE +81-3-5841-4723 #STUDY ST:STUDY_TITLE Quantification of ω-3 fatty acids and their derivatives in lungs from ST:STUDY_TITLE hypoxia-induced pulmonary hypertension (PH) mice. ST:STUDY_SUMMARY Using a liquid chromatography tandem mass spectrometry (LC-MS/MS) system, we ST:STUDY_SUMMARY quantified the ω-3 fatty acid (EPA and DHA) metabolites in the lung tissues of ST:STUDY_SUMMARY mice with PH induced by chronic hypoxia (10% oxygen concentration). ST:INSTITUTE University of Tokyo ST:LAST_NAME Kono ST:FIRST_NAME Nozomu ST:ADDRESS 7-3-1, Hongo, Bunkyo-ku, Tokyo 113-0033, Japan ST:EMAIL nozomu@mol.f.u-tokyo.ac.jp ST:PHONE +81-3-5841-4723 #SUBJECT SU:SUBJECT_TYPE Mammal SU:SUBJECT_SPECIES Mus musculus SU:TAXONOMY_ID 10090 SU:GENDER Male #FACTORS #SUBJECT_SAMPLE_FACTORS: SUBJECT(optional)[tab]SAMPLE[tab]FACTORS(NAME:VALUE pairs separated by |)[tab]Raw file names and additional sample data SUBJECT_SAMPLE_FACTORS - Day0-1 Time after hypoxia (days):- RAW_FILE_NAME=Data180501 lung oxFFA-0d1 SUBJECT_SAMPLE_FACTORS - Day0-2 Time after hypoxia (days):- RAW_FILE_NAME=Data180501 lung oxFFA-0d2 SUBJECT_SAMPLE_FACTORS - Day0-3 Time after hypoxia (days):- RAW_FILE_NAME=Data180501 lung oxFFA-0d3 SUBJECT_SAMPLE_FACTORS - Day4-1 Time after hypoxia (days):4 RAW_FILE_NAME=Data180501 lung oxFFA-4d1 SUBJECT_SAMPLE_FACTORS - Day4-2 Time after hypoxia (days):4 RAW_FILE_NAME=Data180501 lung oxFFA-4d2 SUBJECT_SAMPLE_FACTORS - Day4-3 Time after hypoxia (days):4 RAW_FILE_NAME=Data180501 lung oxFFA-4d3 SUBJECT_SAMPLE_FACTORS - Day14-1 Time after hypoxia (days):14 RAW_FILE_NAME=Data180501 lung oxFFA-14d1 SUBJECT_SAMPLE_FACTORS - Day14-2 Time after hypoxia (days):14 RAW_FILE_NAME=Data180501 lung oxFFA-14d2 SUBJECT_SAMPLE_FACTORS - Day14-3 Time after hypoxia (days):14 RAW_FILE_NAME=Data180501 lung oxFFA-14d3 SUBJECT_SAMPLE_FACTORS - Day28-1 Time after hypoxia (days):28 RAW_FILE_NAME=Data180501 lung oxFFA-28d1 SUBJECT_SAMPLE_FACTORS - Day28-2 Time after hypoxia (days):28 RAW_FILE_NAME=Data180501 lung oxFFA-28d2 SUBJECT_SAMPLE_FACTORS - Day28-3 Time after hypoxia (days):28 RAW_FILE_NAME=Data180501 lung oxFFA-28d3 #COLLECTION CO:COLLECTION_SUMMARY Wild-type male mice (C57BL/6J) were anaesthetized and tissues were harvested. CO:COLLECTION_SUMMARY Isolated mouse tissues were rinsed with cold PBS and immediately frozen in CO:COLLECTION_SUMMARY liquid nitrogen. CO:SAMPLE_TYPE Lung #TREATMENT TR:TREATMENT_SUMMARY In chronic hypoxia mice model, the male mice were housed in a hypoxic chamber TR:TREATMENT_SUMMARY (10 % O2) maintained using a hypoxic air generator (TEIJIN) and monitored with TR:TREATMENT_SUMMARY an O2 analyzer (JIKO-255), for 4, 14 or 28 day. Animals were fed a standard TR:TREATMENT_SUMMARY diet. #SAMPLEPREP SP:SAMPLEPREP_SUMMARY Lipids of tissues were extracted by the method of Bligh and Dyer. The extracted SP:SAMPLEPREP_SUMMARY solutions were dried up with centrifugal evaporator, dissolved in methanol : SP:SAMPLEPREP_SUMMARY isopropanol=1:1, and stored at −20°C. Fatty acid metabolites were further SP:SAMPLEPREP_SUMMARY purified from tissues by solid-phase extraction using InertSep NH2 columns (GL SP:SAMPLEPREP_SUMMARY Science) with deuterium-labelled internal standard (11(12)-EET-d11). Briefly, SP:SAMPLEPREP_SUMMARY InertSep NH2 columns were precon- ditioned with 6mL of hexane and lipids SP:SAMPLEPREP_SUMMARY extracted from tissues by the method of Bligh and Dyer were applied with 500μL SP:SAMPLEPREP_SUMMARY of chloroform. Columns were then washed with 6mL of chloro- form/isopropanol SP:SAMPLEPREP_SUMMARY (2/1, v/v), followed by the elution with diethyl ether/acetic acid (98/2, SP:SAMPLEPREP_SUMMARY v/v).The extracted solutions were dried up with centrifugal evaporator, SP:SAMPLEPREP_SUMMARY dissolved in methanol:isopro- panol=1:1, and stored at −20°C. For the SP:SAMPLEPREP_SUMMARY detection of fatty acid metabolites, chromatographic separation was performed on SP:SAMPLEPREP_SUMMARY a ACQUITY UPLC HSS T3 column (2.1×100 mm, 1.8 µm; Waters) maintained at SP:SAMPLEPREP_SUMMARY 40°C using mobile phase A (water/acetic acid (100/0.1, v/v) containing 10 mM SP:SAMPLEPREP_SUMMARY ammonium acetate) and mobile phase B (acetonitrile/methanol (4/1, v/v) SP:SAMPLEPREP_SUMMARY containing 10 mM ammonium acetate) in a gradient programme (0–2 min: 90% SP:SAMPLEPREP_SUMMARY A; 2–10 min: 90% A →30% A; 10–24 min: 30% A →27% A; 24–27 min: SP:SAMPLEPREP_SUMMARY 1% A; 27–32 min: 90% A) with a flow rate of 0.2 mL/min(0–10 min), SP:SAMPLEPREP_SUMMARY 0.1 mL/min(10–15 min),0.2 mL/min(15–24 min) and SP:SAMPLEPREP_SUMMARY 0.5 mL/min(24–32 min). #CHROMATOGRAPHY CH:CHROMATOGRAPHY_TYPE Reversed phase CH:INSTRUMENT_NAME Shimadzu Nexera UC/s system (Shimadzu) CH:COLUMN_NAME ACQUITY UPLC HSS T3 column (2.1×100 mm, 1.8 µm; Waters) CH:FLOW_GRADIENT mobile phase A (water/acetic acid (100/0.1, v/v) containing 10 mM ammonium CH:FLOW_GRADIENT acetate) and mobile phase B (acetonitrile/methanol (4/1, v/v) containing 10 mM CH:FLOW_GRADIENT ammonium acetate) in a gradient programme (0–2 min: 90% A; 2–10 min: 90% CH:FLOW_GRADIENT A →30% A; 10–24 min: 30% A →27% A; 24–27 min: 1% A; 27–32 min: CH:FLOW_GRADIENT 90% A) with a flow rate of 0.2 mL/min(0–10 min), CH:FLOW_GRADIENT 0.1 mL/min(10–15 min),0.2 mL/min(15–24 min) and CH:FLOW_GRADIENT 0.5 mL/min(24–32 min). CH:FLOW_RATE (0–2 min: 90% A; 2–10 min: 90% A →30% A; 10–24 min: 30% A →27% CH:FLOW_RATE A; 24–27 min: 1% A; 27–32 min: 90% A) with a flow rate of CH:FLOW_RATE 0.2 mL/min(0–10 min), 0.1 mL/min(10–15 min),0.2 CH:FLOW_RATE mL/min(15–24 min) and 0.5 mL/min(24–32 min) CH:COLUMN_TEMPERATURE 40 CH:SOLVENT_A water/acetic acid (100/0.1, v/v) containing 10 mM ammonium acetate CH:SOLVENT_B acetonitrile/methanol (4/1, v/v) containing 10 mM ammonium acetate #ANALYSIS AN:ANALYSIS_TYPE MS #MS MS:INSTRUMENT_NAME ABI Sciex 4500 Qtrap MS:INSTRUMENT_TYPE Ion trap MS:MS_TYPE ESI MS:ION_MODE NEGATIVE MS:MS_COMMENTS The instrument parameters of QTRAP4500 for negative ion mode were as follows: MS:MS_COMMENTS curtain gas, 10 psi; ionspray voltage, −4500 V; temperature, 600°C; ion MS:MS_COMMENTS source gas 1, 70 psi; ion source gas 2, 80 psi. and quantification was performed MS:MS_COMMENTS using MultiQuant™ software (SCIEX). #MS_METABOLITE_DATA MS_METABOLITE_DATA:UNITS ng/mg tissue MS_METABOLITE_DATA_START Samples Day0-1 Day0-2 Day0-3 Day4-1 Day4-2 Day4-3 Day14-1 Day14-2 Day14-3 Day28-1 Day28-2 Day28-3 Factors Time after hypoxia (days):- Time after hypoxia (days):- Time after hypoxia (days):- Time after hypoxia (days):4 Time after hypoxia (days):4 Time after hypoxia (days):4 Time after hypoxia (days):14 Time after hypoxia (days):14 Time after hypoxia (days):14 Time after hypoxia (days):28 Time after hypoxia (days):28 Time after hypoxia (days):28 AA 1.332629635 0.691612138 1.420201592 0.87920638 1.158197869 1.625707737 1.35077187 1.096946827 0.823199611 0.816248741 0.876105027 1.030799112 EPA 0.150560071 0.054815096 0.113585988 0.0914062 0.101475505 0.091695302 0.121606737 0.088131893 0.080014934 0.090599818 0.073905628 0.07760927 DHA 1.309128582 0.679975966 0.837107885 0.888611198 0.941862326 1.082425218 0.835055096 0.665564738 0.571522553 0.882320074 0.546255092 0.737319721 5-HETE 0.196337935 0.163000925 0.231701085 0.149322731 0.133177392 0.1962096 0.126471413 0.183318386 0.156759444 0.218673419 0.176760459 0.221200588 8-HETE 0.001193885 0.002850373 0.001668369 0.001145624 0.001776613 0.00176225 0.001144255 0.001040577 0.001838212 0.001204792 0.001767122 0.001430269 9-HETE 0.010400255 0.009260183 0.009241666 0.006757653 0.009144106 0.011214914 0.011252245 0.011488776 0.007357704 0.008371222 0.009458246 0.010475905 11-HETE 0.006135379 0.003856802 0.004139105 0.00290529 0.003506085 0.017565401 0.007474203 0.01429298 0.002407256 0.006604251 0.005071509 0.014177479 12-HETE 0.026198439 0.008603209 0.058206228 0.011977688 0.007578779 0.046449489 0.012712611 0.019220612 0.005583195 0.012198707 0.008094884 0.019430236 15-HETE 0.20539058 0.128638245 0.193784071 0.103842759 0.143647033 0.42692801 0.223532806 0.351740347 0.10172974 0.162460806 0.134604623 0.330779486 16-HETE 0.000316032 0.000804494 0.000401673 0.000558456 0.00045047 0.00056043 0.000497206 0.000412363 0.000517881 0.000546159 0.000427448 0.000397052 17-HETE 0.000888794 0.000518758 0.000605069 0.000734795 0.000701998 0.000903858 0.000543285 0.000810252 0.000521084 0.000730981 0.00061419 0.000739482 18-HETE 0.001139068 0.000910515 0.001025649 0.001150089 0.000850997 0.000834178 0.000787392 0.000849545 0.000548019 0.001103448 0.000765411 0.000848986 19-HETE 0.004979492 0.00923135 0.011477702 0.009097368 0.009411751 0.006755135 0.007600561 0.00606174 0.006292206 0.006152217 0.006687295 0.007190154 20-HETE 0.005338916 0.002692067 0.002759803 0.002708477 0.003385459 0.002484171 0.001697161 0.002385226 0.00208261 0.002427638 0.001893613 0.00231502 5,6-EET 0.010792737 0.009603636 0.016191675 0.010428423 0.006006967 0.007519985 0.004347027 0.007083841 0.002223595 0.006967584 0.009248873 0.006547965 8,9-EET 0.003958708 0.004638982 0.005820906 0.005603249 0.004695024 0.005277554 0.006030303 0.00521503 0.004085029 0.003676768 0.004921212 0.003602496 11,12-EET 0.002094514 0.002732497 0.002310557 0.001986864 0.002257773 0.002248735 0.002022885 0.001690887 0.001693209 0.00174947 0.001761026 0.00188406 14,15-EET 0.003323461 0.003312913 0.003701922 0.003348135 0.003597316 0.003539823 0.002514956 0.002811755 0.002957505 0.002664161 0.003398566 0.00252877 5,6-DHET 0.001036644 0.000312633 0.000675006 0.00040921 0.000679564 0.000469119 0.000756082 0.000711309 0.000568696 0.00048208 0.000963547 0.000631886 8,9-DHET 0.000914492 0.000443639 0.000813278 0.000406313 0.000337838 0.000770325 0.000466707 0.000522119 0.000590457 0.000400302 0.000727654 0.000605758 11,12-DHET 0.000341166 0.000441905 0.000323266 0.000375622 0.000340215 0.000403358 0.000361373 0.000261501 0.00025319 0.000379297 0.000265099 0.000571349 14,15-DHET 0.000531924 0.000448375 0.000552092 0.000683728 0.000529682 0.000458196 0.000559588 0.000536267 0.000483348 0.00063985 0.000473683 0.001031458 5-HEPE 0.001447606 0.001710222 0.002347177 0.001673675 0.001109447 0.003385066 0.00208218 0.001990481 0.000877847 0.00127476 0.001173386 0.001521534 8-HEPE 0.002772061 0.002363133 0.002564892 0.002556335 0.002827671 0.001678206 0.002402156 0.002495337 0.001668195 0.001788211 0.002118089 0.0016306 9-HEPE 0.001352618 0.001092199 0.001304001 0.00111686 0.001808018 0.002184646 0.001188491 0.001815392 0.001574559 0.00115857 0.001229407 0.001509459 11-HEPE 0.001475127 0.001469387 0.001682758 0.001282885 0.001474392 0.00174132 0.001465607 0.001513288 0.001291095 0.001492179 0.001078286 0.001373264 12-HEPE 0.003572782 0.001838168 0.005180716 0.002188817 0.002050662 0.004363747 0.001739532 0.002563547 0.002014558 0.002265619 0.001786662 0.003169371 15-HEPE 0.000904339 0.00184965 0.00096501 0.001109136 0.001216333 0.001375312 0.000918271 0.001410702 0.000861182 0.000792707 0.00077545 0.002283696 18-HEPE 0.001444015 0.001443013 0.002335408 0.001635326 0.001451226 0.001632474 0.00141098 0.00161654 0.001150352 0.001008325 0.001248982 0.001525061 19-HEPE 0.029225129 0.083058922 0.119311218 0.07030342 0.056340871 0.047573469 0.040387259 0.035714024 0.029583977 0.028123318 0.02674681 0.027393244 20-HEPE 0.002691242 0.00300617 0.002675669 0.002079726 0.002257418 0.002766263 0.00104919 0.001750557 0.001792523 0.001415666 0.002601352 0.002726931 8,9-EpETE 0.001098563 0.000818829 0.001157783 0.001102431 0.00109103 0.000701908 0.00099135 0.000865649 0.000895431 0.000961715 0.000914629 0.00119699 11,12-EpETE 0.000324572 0.000390902 0.000329246 0.000267997 0.000234695 0.000222471 0.000411165 0.000440067 0.000262108 0.000394276 0.000418382 0.000248597 14,15-EpETE 0.000371648 0.000402217 0.000748776 0.000475064 0.000465161 0.00039245 0.000685373 0.000644303 0.000449973 0.000376875 0.000731234 0.000365145 17,18-EpETE 0.007099365 0.007656601 0.01136047 0.006129804 0.007776379 0.005777897 0.007831052 0.005249604 0.007029496 0.005512627 0.005666734 0.005516646 17,18-diHETE 0.029625564 0.021063093 0.022956876 0.018348716 0.014428852 0.0151627 0.01313576 0.014122211 0.010075713 0.012197281 0.010456614 0.015704342 4-HDoHE 0.003697283 0.002400365 0.002536101 0.001910938 0.002097336 0.001345377 0.001486951 0.001752228 0.001229813 0.001778994 0.001506239 0.001638356 7-HDoHE 0.001271772 0.001384278 0.001321313 0.001110957 0.00100417 0.001582427 0.001474802 0.001286324 0.000782137 0.001496957 0.000842445 0.001243897 8-HDoHE 0.003489205 0.002988734 0.004622431 0.004301688 0.004429032 0.003267222 0.003355959 0.003863018 0.003800602 0.004012358 0.003832049 0.00498631 10-HDoHE 0.002323813 0.002673189 0.001893541 0.001739818 0.003115421 0.001585152 0.001593392 0.001720838 0.002363037 0.001184357 0.001101074 0.001746215 11-HDoHE 0.001482286 0.001977382 0.001507211 0.001506963 0.001521635 0.001640305 0.001143453 0.001570896 0.001177879 0.001314854 0.001479621 0.001902711 13-HDoHE 0.010225919 0.010360634 0.011132579 0.012901842 0.010054564 0.011995851 0.010020194 0.010767141 0.009311602 0.009588136 0.009776729 0.009530636 14-HDoHE 0.0050382 0.006478542 0.003428571 0.004361316 0.006570555 0.008372524 0.002477679 0.003302095 0.003341862 0.005587302 0.003037363 0.016134454 17-HDoHE 0.002276999 0.003583841 0.002500376 0.002100465 0.003487827 0.003751488 0.002044896 0.002711566 0.001600338 0.002517703 0.001589058 0.007735919 16-HDoHE 0.001179098 0.002087149 0.001164256 0.00080584 0.001686015 0.001255911 0.000744496 0.000696261 0.000940262 0.000834817 0.000748817 0.00143511 20-HDoHE 0.001858111 0.00217719 0.002382648 0.001818066 0.001912851 0.001924471 0.001612007 0.001811437 0.001299915 0.001490395 0.001237665 0.001842213 21-HDoHE 0.006542104 0.016889719 0.017522215 0.020156516 0.02246036 0.017252919 0.015639589 0.020855275 0.019719331 0.016702977 0.019478561 0.021283023 22-HDoHE 0.009793878 0.002946921 0.003056561 0.004706156 0.00505883 0.004101045 0.003899629 0.003827119 0.003655452 0.003403282 0.002968275 0.002629611 16,17-EpDPE 0.00204749 0.002122042 0.001956219 0.001907502 0.001653411 0.001959662 0.002391405 0.002014048 0.001660827 0.001411114 0.001464524 0.001958519 19,20-EpDPE 0.003899079 0.003341083 0.004002406 0.003487831 0.003598926 0.003211723 0.003495037 0.004068782 0.002923312 0.003159957 0.00339395 0.003704739 19,20-diHDoPE 0.017859887 0.010200106 0.014041577 0.010659374 0.008694154 0.007764134 0.0084586 0.007498202 0.007048259 0.009341172 0.007683088 0.007332378 MS_METABOLITE_DATA_END #METABOLITES METABOLITES_START metabolite_name Pubchem ID Q1 Mass (Da) Q3 Mass (Da) AA 444899 303 259 EPA 446284  301 257 DHA 445580 327.1 283 5-HETE 5280733 319 115 8-HETE 11976122 319.01 155 9-HETE 14123398 319.02 123 11-HETE 14123410 319.03 167 12-HETE 5353272 319.04 179 15-HETE 9966861 319.05 219 16-HETE 6442739 319.06 233 17-HETE 6442740  319.07 247 18-HETE 6442778 319.08 261 19-HETE  20839325   319.09 231 20-HETE 5283157 319.1 245 5,6-EET 5283202 319.11 191 8,9-EET  5283203  319.12 155 11,12-EET  5283204 319.13 167 14,15-EET  5283205 319.14 219 5,6-DHET 5283142 337 145 8,9-DHET 5283144 337.01 127 11,12-DHET  5283146 337.02 167 14,15-DHET 5283147   337.03 207 5-HEPE  6439678 317.2 115 8-HEPE 16061128  317.21 155 9-HEPE 122164870   317.21 149 11-HEPE  16061130 317.21 167 12-HEPE 10041593  317.2 179 15-HEPE 16061131 317.2 219 18-HEPE 16061132 317.21 259 19-HEPE 72551575 317.2 229 20-HEPE 72551579  317.2 287 8,9-EpETE 16061086 317.2 155 11,12-EpETE 16061087 317.2 167 14,15-EpETE 16061088  317.2 207 17,18-EpETE  6439311  317.2 259 17,18-diHETE 16061120  335 247 4-HDoHE 14429109 343.1 101 7-HDoHE 16061142  343.1 141 8-HDoHE 11976798  343.1 109 10-HDoHE 11537494  343.1 153 11-HDoHE 11631564  343.1 149 13-HDoHE 11559259 343.1 221 14-HDoHE 11566378  343.1 205 17-HDoHE 6439179 343.1 201 16-HDoHE 11595378  343.11 233 20-HDoHE 16061143  343.11 241 21-HDoHE 52922000 343.1 255 22-HDoHE NA 343.1 269 16,17-EpDPE 14392758 343.1 233 19,20-EpDPE 11631565 343.1 241 19,20-diHDoPE  16061148 361.1 273.1 METABOLITES_END #END