#METABOLOMICS WORKBENCH Zhulab_20221116_105018 DATATRACK_ID:3579 STUDY_ID:ST002378 ANALYSIS_ID:AN003876
VERSION                          	1
CREATED_ON                       	12-15-2022
#PROJECT
PR:PROJECT_TITLE                 	Pyruvate dehydrogenase kinase supports macrophage NLRP3 inflammasome activation
PR:PROJECT_TITLE                 	during acute inflammation
PR:PROJECT_TYPE                  	Basic research
PR:PROJECT_SUMMARY               	Activating macrophage NLRP3 inflammasome can promote excessive inflammation,
PR:PROJECT_SUMMARY               	with severe cell and tissue damage and organ dysfunction. Here, we show that
PR:PROJECT_SUMMARY               	pharmacological or genetic inhibition of pyruvate dehydrogenase kinase (PDHK)
PR:PROJECT_SUMMARY               	significantly attenuates NLRP3 inflammasome activation in murine and human
PR:PROJECT_SUMMARY               	macrophages and septic mice by lowering caspase-1 cleavage and IL-1beta
PR:PROJECT_SUMMARY               	secretion. Inhibiting PDHK reverses NLRP3 inflammasome-induced metabolic
PR:PROJECT_SUMMARY               	reprogramming, enhances autophagy, promotes mitochondrial fusion over fission,
PR:PROJECT_SUMMARY               	preserves cristae ultrastructure, and attenuates mitochondrial ROS production.
PR:PROJECT_SUMMARY               	The suppressive effect of PDHK inhibition on the NLRP3 inflammasome is
PR:PROJECT_SUMMARY               	independent of its canonical role as a pyruvate dehydrogenase regulator. We
PR:PROJECT_SUMMARY               	suggest that PDHK inhibition improves mitochondrial fitness by reversing NLRP3
PR:PROJECT_SUMMARY               	inflammasome activation in acutely inflamed macrophages.
PR:INSTITUTE                     	Wake Forest School of Medicine
PR:LAST_NAME                     	Zhu
PR:FIRST_NAME                    	Xuewei
PR:ADDRESS                       	575 Patterson Ave
PR:EMAIL                         	xwzhu@wakehealth.edu
PR:PHONE                         	3367131445
PR:DOI                           	http://dx.doi.org/10.21228/M8Q13W
#STUDY
ST:STUDY_TITLE                   	Targeted metabolomics analysis of WT and GSDMDKO macrophages
ST:STUDY_TYPE                    	MS analysis
ST:STUDY_SUMMARY                 	Activating macrophage NLRP3 inflammasome can promote excessive inflammation,
ST:STUDY_SUMMARY                 	with severe cell and tissue damage and organ dysfunction. Here, we show that
ST:STUDY_SUMMARY                 	pharmacological or genetic inhibition of pyruvate dehydrogenase kinase (PDHK)
ST:STUDY_SUMMARY                 	significantly attenuates NLRP3 inflammasome activation in murine and human
ST:STUDY_SUMMARY                 	macrophages and septic mice by lowering caspase-1 cleavage and IL-1beta
ST:STUDY_SUMMARY                 	secretion. Inhibiting PDHK reverses NLRP3 inflammasome-induced metabolic
ST:STUDY_SUMMARY                 	reprogramming, enhances autophagy, promotes mitochondrial fusion over fission,
ST:STUDY_SUMMARY                 	preserves cristae ultrastructure, and attenuates mitochondrial ROS production.
ST:STUDY_SUMMARY                 	The suppressive effect of PDHK inhibition on the NLRP3 inflammasome is
ST:STUDY_SUMMARY                 	independent of its canonical role as a pyruvate dehydrogenase regulator. We
ST:STUDY_SUMMARY                 	suggest that PDHK inhibition improves mitochondrial fitness by reversing NLRP3
ST:STUDY_SUMMARY                 	inflammasome activation in acutely inflamed macrophages.
ST:INSTITUTE                     	Wake Forest School of Medicine
ST:LAST_NAME                     	Zhu
ST:FIRST_NAME                    	Xuewei
ST:ADDRESS                       	575 Patterson Ave, Winston-Salem, NC 27101
ST:EMAIL                         	xwzhu@wakehealth.edu
ST:PHONE                         	3367131445
ST:SUBMIT_DATE                   	2022-11-16
#SUBJECT
SU:SUBJECT_TYPE                  	Cultured cells
SU:SUBJECT_SPECIES               	Mus musculus
SU:TAXONOMY_ID                   	10090
SU:GENDER                        	Male and female
#SUBJECT_SAMPLE_FACTORS:         	SUBJECT(optional)[tab]SAMPLE[tab]FACTORS(NAME:VALUE pairs separated by |)[tab]Additional sample data
SUBJECT_SAMPLE_FACTORS           	-	GSDMD-LPS-1	Genotype:GSDMDKO | Treatment:LPS	RAW_FILE_NAME=GSDMD-LPS-1.mzml
SUBJECT_SAMPLE_FACTORS           	-	GSDMD-LPS-2	Genotype:GSDMDKO | Treatment:LPS	RAW_FILE_NAME=GSDMD-LPS-2.mzml
SUBJECT_SAMPLE_FACTORS           	-	GSDMD-LPS-3	Genotype:GSDMDKO | Treatment:LPS	RAW_FILE_NAME=GSDMD-LPS-3.mzml
SUBJECT_SAMPLE_FACTORS           	-	GSDMD-LPS-4	Genotype:GSDMDKO | Treatment:LPS	RAW_FILE_NAME=GSDMD-LPS-4.mzml
SUBJECT_SAMPLE_FACTORS           	-	GSDMD-ATP-1	Genotype:GSDMDKO | Treatment:LPS+ATP	RAW_FILE_NAME=GSDMD-ATP-1.mzml
SUBJECT_SAMPLE_FACTORS           	-	GSDMD-ATP-2	Genotype:GSDMDKO | Treatment:LPS+ATP	RAW_FILE_NAME=GSDMD-ATP-2.mzml
SUBJECT_SAMPLE_FACTORS           	-	GSDMD-ATP-3	Genotype:GSDMDKO | Treatment:LPS+ATP	RAW_FILE_NAME=GSDMD-ATP-3.mzml
SUBJECT_SAMPLE_FACTORS           	-	GSDMD-ATP-4	Genotype:GSDMDKO | Treatment:LPS+ATP	RAW_FILE_NAME=GSDMD-ATP-4.mzml
SUBJECT_SAMPLE_FACTORS           	-	GSDMD-JX-1	Genotype:GSDMDKO | Treatment:LPS+JX06+ATP	RAW_FILE_NAME=GSDMD-JX-1.mzml
SUBJECT_SAMPLE_FACTORS           	-	GSDMD-JX-2	Genotype:GSDMDKO | Treatment:LPS+JX06+ATP	RAW_FILE_NAME=GSDMD-JX-2.mzml
SUBJECT_SAMPLE_FACTORS           	-	GSDMD-JX-3	Genotype:GSDMDKO | Treatment:LPS+JX06+ATP	RAW_FILE_NAME=GSDMD-JX-3.mzml
SUBJECT_SAMPLE_FACTORS           	-	GSDMD-JX-4	Genotype:GSDMDKO | Treatment:LPS+JX06+ATP	RAW_FILE_NAME=GSDMD-JX-4.mzml
SUBJECT_SAMPLE_FACTORS           	-	GSDMD-control-1	Genotype:GSDMDKO | Treatment:no treatment	RAW_FILE_NAME=GSDMD-control-1.mzml
SUBJECT_SAMPLE_FACTORS           	-	GSDMD-control-2	Genotype:GSDMDKO | Treatment:no treatment	RAW_FILE_NAME=GSDMD-control-2.mzml
SUBJECT_SAMPLE_FACTORS           	-	GSDMD-control-3	Genotype:GSDMDKO | Treatment:no treatment	RAW_FILE_NAME=GSDMD-control-3.mzml
SUBJECT_SAMPLE_FACTORS           	-	GSDMD-control-4	Genotype:GSDMDKO | Treatment:no treatment	RAW_FILE_NAME=GSDMD-control-4.mzml
SUBJECT_SAMPLE_FACTORS           	-	WT-LPS-1	Genotype:WT | Treatment:LPS	RAW_FILE_NAME=WT-LPS-1.mzml
SUBJECT_SAMPLE_FACTORS           	-	WT-LPS-2	Genotype:WT | Treatment:LPS	RAW_FILE_NAME=WT-LPS-2.mzml
SUBJECT_SAMPLE_FACTORS           	-	WT-LPS-3	Genotype:WT | Treatment:LPS	RAW_FILE_NAME=WT-LPS-3.mzml
SUBJECT_SAMPLE_FACTORS           	-	WT-LPS-4	Genotype:WT | Treatment:LPS	RAW_FILE_NAME=WT-LPS-4.mzml
SUBJECT_SAMPLE_FACTORS           	-	WT-ATP-1	Genotype:WT | Treatment:LPS+ATP	RAW_FILE_NAME=WT-ATP-1.mzml
SUBJECT_SAMPLE_FACTORS           	-	WT-ATP-2	Genotype:WT | Treatment:LPS+ATP	RAW_FILE_NAME=WT-ATP-2.mzml
SUBJECT_SAMPLE_FACTORS           	-	WT-ATP-3	Genotype:WT | Treatment:LPS+ATP	RAW_FILE_NAME=WT-ATP-3.mzml
SUBJECT_SAMPLE_FACTORS           	-	WT-ATP-4	Genotype:WT | Treatment:LPS+ATP	RAW_FILE_NAME=WT-ATP-4.mzml
SUBJECT_SAMPLE_FACTORS           	-	WT-JX-1	Genotype:WT | Treatment:LPS+JX06+ATP	RAW_FILE_NAME=WT-JX-1.mzml
SUBJECT_SAMPLE_FACTORS           	-	WT-JX-2	Genotype:WT | Treatment:LPS+JX06+ATP	RAW_FILE_NAME=WT-JX-2.mzml
SUBJECT_SAMPLE_FACTORS           	-	WT-JX-3	Genotype:WT | Treatment:LPS+JX06+ATP	RAW_FILE_NAME=WT-JX-3.mzml
SUBJECT_SAMPLE_FACTORS           	-	WT-JX-4	Genotype:WT | Treatment:LPS+JX06+ATP	RAW_FILE_NAME=WT-JX-4.mzml
SUBJECT_SAMPLE_FACTORS           	-	WT-control-1	Genotype:WT | Treatment:no treatment	RAW_FILE_NAME=WT-control-1.mzml
SUBJECT_SAMPLE_FACTORS           	-	WT-control-2	Genotype:WT | Treatment:no treatment	RAW_FILE_NAME=WT-control-2.mzml
SUBJECT_SAMPLE_FACTORS           	-	WT-control-3	Genotype:WT | Treatment:no treatment	RAW_FILE_NAME=WT-control-3.mzml
SUBJECT_SAMPLE_FACTORS           	-	WT-control-4	Genotype:WT | Treatment:no treatment	RAW_FILE_NAME=WT-control-4.mzml
#COLLECTION
CO:COLLECTION_SUMMARY            	Macrophages were lysed, and polar metabolites were extracted using methanol and
CO:COLLECTION_SUMMARY            	H2O (80:20; HPLC Grade; Sigma-Aldrich). Briefly, After treatment, immediately
CO:COLLECTION_SUMMARY            	aspirate medium at room temperature. Immediately place the plate on dry ice, and
CO:COLLECTION_SUMMARY            	add 1 mL 80% methanol/water (both HPLC grade) (pre-cooled in -80oC for at least
CO:COLLECTION_SUMMARY            	1hr).Remove the plate from -80oC freezer and put it on dry ice, scrape cells
CO:COLLECTION_SUMMARY            	into extraction solvent. Transfer the whole cell extract to a new Eppendorf tube
CO:COLLECTION_SUMMARY            	placed on ice. Centrifuge at 20 000 rcf for 10 min, 4oC.Transfer the supernatant
CO:COLLECTION_SUMMARY            	into two tubes and dry with a speed vacuum at room temperature.
CO:SAMPLE_TYPE                   	Macrophages
CO:STORAGE_CONDITIONS            	Described in summary
#TREATMENT
TR:TREATMENT_SUMMARY             	WT and GSDMD KO bone marrow derived macrophages were first primed with 300 ng/ml
TR:TREATMENT_SUMMARY             	LPS (E. coli 0111; B4, Sigma-Aldrich) before stimulated with or without 5 mM ATP
TR:TREATMENT_SUMMARY             	(Sigma-Aldrich) for 30 min in the presence or absence of 10 uM JX06. Here, we
TR:TREATMENT_SUMMARY             	show that pharmacological or genetic inhibition of pyruvate dehydrogenase kinase
TR:TREATMENT_SUMMARY             	(PDHK) significantly attenuates NLRP3 inflammasome activation in murine and
TR:TREATMENT_SUMMARY             	human macrophages and septic mice by lowering caspase-1 cleavage and IL-1beta
TR:TREATMENT_SUMMARY             	secretion. Inhibiting PDHK reverses NLRP3 inflammasome-induced metabolic
TR:TREATMENT_SUMMARY             	reprogramming, enhances autophagy, promotes mitochondrial fusion over fission,
TR:TREATMENT_SUMMARY             	preserves cristae ultrastructure, and attenuates mitochondrial ROS production.
TR:TREATMENT_SUMMARY             	The suppressive effect of PDHK inhibition on the NLRP3 inflammasome is
TR:TREATMENT_SUMMARY             	independent of its canonical role as a pyruvate dehydrogenase regulator. We
TR:TREATMENT_SUMMARY             	suggest that PDHK inhibition improves mitochondrial fitness by reversing NLRP3
TR:TREATMENT_SUMMARY             	inflammasome activation in acutely inflamed macrophages.
TR:TREATMENT                     	In vitro culture
TR:TREATMENT_COMPOUND            	LPS, ATP, JX06
#SAMPLEPREP
SP:SAMPLEPREP_SUMMARY            	Macrophages were lysed, and polar metabolites were extracted using methanol and
SP:SAMPLEPREP_SUMMARY            	H2O (80:20; HPLC Grade; Sigma-Aldrich). Briefly, After treatment, immediately
SP:SAMPLEPREP_SUMMARY            	aspirate medium at room temperature. Immediately place the plate on dry ice, and
SP:SAMPLEPREP_SUMMARY            	add 1 mL 80% methanol/water (both HPLC grade) (pre-cooled in -80oC for at least
SP:SAMPLEPREP_SUMMARY            	1hr).Remove the plate from -80oC freezer and put it on dry ice, scrape cells
SP:SAMPLEPREP_SUMMARY            	into extraction solvent. Transfer the whole cell extract to a new Eppendorf tube
SP:SAMPLEPREP_SUMMARY            	placed on ice. Centrifuge at 20 000 rcf for 10 min, 4oC.Transfer the supernatant
SP:SAMPLEPREP_SUMMARY            	into two tubes and dry with a speed vacuum at room temperature. The dried
SP:SAMPLEPREP_SUMMARY            	metabolites were stored at -80 freezer before analysis.
SP:PROCESSING_STORAGE_CONDITIONS 	Described in summary
SP:EXTRACT_STORAGE               	Described in summary
#CHROMATOGRAPHY
CH:CHROMATOGRAPHY_SUMMARY        	PFPP A gradient separation on a Restek Ultra PFPP column (150 x 2.1 mm, 3 μm;
CH:CHROMATOGRAPHY_SUMMARY        	Restek, Bellefonte, PA) was used to separate the analytes. Mobile phase A
CH:CHROMATOGRAPHY_SUMMARY        	consisted of 0.1% formic acid in water and mobile phase B consisted of 0.1%
CH:CHROMATOGRAPHY_SUMMARY        	formic acid in 100% acetonitrile. The gradient began with 2 minutes at 0% B
CH:CHROMATOGRAPHY_SUMMARY        	followed by a ramp to 25% B between 2 and 5 minutes, another ramp to 35% B
CH:CHROMATOGRAPHY_SUMMARY        	between 5 and 11 minutes, a final increase from 35% to 95% B between 11 and 15
CH:CHROMATOGRAPHY_SUMMARY        	minutes, a hold at 95% B from 15 to 20 minutes, then a decrease to 0% B between
CH:CHROMATOGRAPHY_SUMMARY        	20 and 20.10 minutes, and a final hold at 0% B from 20.10 to 25 minutes. The
CH:CHROMATOGRAPHY_SUMMARY        	flow rate to achieve separation was 0.25 ml/min. Ionization in the negative ESI
CH:CHROMATOGRAPHY_SUMMARY        	mode occurred in the DUIS source with the following conditions: nebulizing gas
CH:CHROMATOGRAPHY_SUMMARY        	flow of 2 L/min, heating gas flow of 5 L/min, interface temperature of 350°C,
CH:CHROMATOGRAPHY_SUMMARY        	DL temperature of 250°C, heat block temperature of 400°C, and a drying gas
CH:CHROMATOGRAPHY_SUMMARY        	flow of 15 L/min.
CH:INSTRUMENT_NAME               	Shimadzu Nexera X2
CH:COLUMN_NAME                   	Restek Ultra PFPP (150 x 2.1mm,3um)
CH:FLOW_GRADIENT                 	The gradient began with 2 minutes at 0% B followed by a ramp to 25% B between 2
CH:FLOW_GRADIENT                 	and 5 minutes, another ramp to 35% B between 5 and 11 minutes, a final increase
CH:FLOW_GRADIENT                 	from 35% to 95% B between 11 and 15 minutes, a hold at 95% B from 15 to 20
CH:FLOW_GRADIENT                 	minutes, then a decrease to 0% B between 20 and 20.10 minutes, and a final hold
CH:FLOW_GRADIENT                 	at 0% B from 20.10 to 25 minutes.
CH:FLOW_RATE                     	0.25 ml/min
CH:SOLVENT_A                     	100% water; 0.1% formic acid
CH:SOLVENT_B                     	100% acetonitrile
CH:CHROMATOGRAPHY_TYPE           	Other
#ANALYSIS
AN:ANALYSIS_TYPE                 	MS
#MS
MS:INSTRUMENT_NAME               	Shimadzu Nexera X2
MS:INSTRUMENT_TYPE               	Triple quadrupole
MS:MS_TYPE                       	ESI
MS:MS_COMMENTS                   	The analysis was performed on a Shimadzu Nexera UHPLC system coupled with a
MS:MS_COMMENTS                   	Shimadzu LCMS-8050 triple-quadrupole mass spectrometer (Kyoto, Japan). Two
MS:MS_COMMENTS                   	LC-MS/MS methods were employed to measure the targets.
MS:ION_MODE                      	NEGATIVE
#MS_METABOLITE_DATA
MS_METABOLITE_DATA:UNITS         	Peak area ratio
MS_METABOLITE_DATA_START
Samples	GSDMD-LPS-1	GSDMD-LPS-2	GSDMD-LPS-3	GSDMD-LPS-4	GSDMD-ATP-1	GSDMD-ATP-2	GSDMD-ATP-3	GSDMD-ATP-4	GSDMD-JX-1	GSDMD-JX-2	GSDMD-JX-3	GSDMD-JX-4	GSDMD-control-1	GSDMD-control-2	GSDMD-control-3	GSDMD-control-4	WT-LPS-1	WT-LPS-2	WT-LPS-3	WT-LPS-4	WT-ATP-1	WT-ATP-2	WT-ATP-3	WT-ATP-4	WT-JX-1	WT-JX-2	WT-JX-3	WT-JX-4	WT-control-1	WT-control-2	WT-control-3	WT-control-4
Factors	Genotype:GSDMDKO | Treatment:LPS	Genotype:GSDMDKO | Treatment:LPS	Genotype:GSDMDKO | Treatment:LPS	Genotype:GSDMDKO | Treatment:LPS	Genotype:GSDMDKO | Treatment:LPS+ATP	Genotype:GSDMDKO | Treatment:LPS+ATP	Genotype:GSDMDKO | Treatment:LPS+ATP	Genotype:GSDMDKO | Treatment:LPS+ATP	Genotype:GSDMDKO | Treatment:LPS+JX06+ATP	Genotype:GSDMDKO | Treatment:LPS+JX06+ATP	Genotype:GSDMDKO | Treatment:LPS+JX06+ATP	Genotype:GSDMDKO | Treatment:LPS+JX06+ATP	Genotype:GSDMDKO | Treatment:no treatment	Genotype:GSDMDKO | Treatment:no treatment	Genotype:GSDMDKO | Treatment:no treatment	Genotype:GSDMDKO | Treatment:no treatment	Genotype:WT | Treatment:LPS	Genotype:WT | Treatment:LPS	Genotype:WT | Treatment:LPS	Genotype:WT | Treatment:LPS	Genotype:WT | Treatment:LPS+ATP	Genotype:WT | Treatment:LPS+ATP	Genotype:WT | Treatment:LPS+ATP	Genotype:WT | Treatment:LPS+ATP	Genotype:WT | Treatment:LPS+JX06+ATP	Genotype:WT | Treatment:LPS+JX06+ATP	Genotype:WT | Treatment:LPS+JX06+ATP	Genotype:WT | Treatment:LPS+JX06+ATP	Genotype:WT | Treatment:no treatment	Genotype:WT | Treatment:no treatment	Genotype:WT | Treatment:no treatment	Genotype:WT | Treatment:no treatment	
Citrate/Isocitrate	7.0220	8.4980	10.9830	8.2710	5.3300	8.3200	12.9110	6.4650	9.7820	11.2200	13.0720	12.5190	2.7060	5.4950	5.0450	8.5770	5.1240	4.8600	4.9040	5.7650	4.5580	8.9670	4.8240	3.2790	10.7510	4.7270	3.9460	3.1670	3.3330	4.5700	2.7730	3.8570
Fumaric Acid	0.0110	0.0100	0.0150	0.0170	0.0150	0.0180	0.0300	0.0140	0.0140	0.0170	0.0210	0.0200	0.0030	0.0050	0.0030	0.0050	0.0100	0.0060	0.0080	0.0100	0.0140	0.0130	0.0110	0.0160	0.0140	0.0090	0.0100	0.0070	0.0040	0.0020	0.0190	0.0050
Lactic Acid	8.2300	7.4980	9.1980	6.5430	2.1950	2.1560	4.2970	1.9870	2.6630	2.6320	3.2420	3.7440	0.8720	1.6990	1.5780	3.2270	3.3380	3.0750	4.4800	5.2680	2.4830	3.5150	3.5750	2.5310	2.3490	1.2450	2.0360	1.6400	0.7810	1.1450	0.9390	1.1040
Malic Acid	0.9580	1.0470	1.4320	1.0950	0.5710	0.9110	1.5560	0.8550	0.8230	0.7710	1.2290	1.3610	0.2050	0.3790	0.4280	0.7730	0.7220	0.6250	0.8200	1.0090	0.6230	1.4860	1.2030	1.0090	1.1010	0.6610	0.9380	0.7510	0.2650	0.3450	0.3960	0.4320
Succinic acid	0.5130	0.4950	0.7190	0.6160	0.4470	0.5350	0.9480	0.4630	0.5050	0.5140	0.6270	0.6480	0.1080	0.1980	0.2310	0.4830	0.5410	0.3790	0.5920	0.7180	0.5010	0.9300	0.8670	0.7570	0.5620	0.2880	0.4570	0.3810	0.1900	0.2220	0.3620	0.2990
MS_METABOLITE_DATA_END
#METABOLITES
METABOLITES_START
metabolite_name	pubchem_id	inchi_key	kegg_id	other_id	other_id_type	ri	ri_type	moverz_quant	
Citrate/Isocitrate	1198		C00311						
Fumaric Acid									
Lactic Acid									
Malic Acid									
Succinic acid									
METABOLITES_END
#END