Abstract The brain is the main oxygen-consuming organ and is vulnerable to ischemic shock or insufficient blood perfusion. Brain hypoxia has a persistent and detrimental effect on resident neurons. Previous studies have identified alterations in genes and metabolites in ischemic brain shock by single omics, but the adaptive systems that neurons use to cope with hypoxia remain uncovered. In the present study, we constructed an acute hypoxia model and performed a multi-omics analysis from RNA-sequencing and liquid chromatography-mass spectrometry (LC-MS)-based metabolomics on exploring potentially differentially expressed genes (DEGs) and metabolites (DEMs) in primary cortical neurons under severe acute hypoxic conditions. The TUNEL assay showed acute hypoxia-induced apoptosis in cortical neurons. Omics analysis identified 564 DEGs and 46 DEMs categorized in the Kyoto encyclopedia of genes and genomes (KEGG) database. Integrative pathway analysis highlighted that dysregulated lipid metabolism, enhanced glycolysis, and activated HIF-1 signaling pathways could regulate neuron physiology and pathophysiology under hypoxia. These findings may help us understand the transcriptional and metabolic mechanisms by which cortical neurons respond to hypoxia and identify potential targets for neuron protection. Keywords: Hypoxia, Neuron, RNA sequencing, Metabolomics, Multi-omics analysis Highlights * • Acute hypoxia induces apoptosis in primary cortical neurons. * • Acute hypoxia alters the metabolomics and transcriptomics profiles of cortical neurons. * • Multi-omics analysis shows dysregulated lipid metabolism, enhanced glycolysis and activated HIF-1 signaling. 1. Introduction The brain is one of the most metabolically active tissues and organs, consuming ∼20% of the total basal oxygen (O[2]) to meet the high energy demands of neuronal activity [[33][1], [34][2], [35][3], [36][4]]. As a highly oxygen-consuming organ, the brain is inherently vulnerable to hypoxia [[37]3,[38]5]. In humans and most mammals, substantially reducing oxygen supply severely impairs brain function [[39][6], [40][7], [41][8], [42][9]], and prolonging hypoxia irreversibly damages the brain structure and function. For example, acute ischemic shock leads to massive neuron death and blood-brain barrier disruption, while inadequate cerebral perfusion induces various neuronal disorders [[43]7,[44][10], [45][11], [46][12]]. The cortex is the most affected brain region during ischemia and neonatal hypoxic-ischemic encephalopathy [[47]13,[48]14]. Cerebral hypoxia can lead to cerebral infarcts that are challenging to recover from or even life-threatening. Although various studies have documented possible mechanisms involving differentially expressed genes (DEGs) and metabolites (DEMs), there is still a lack of effective interventions for ischemia based on current knowledge. In particular, neurons, the primary cell types resident in the brain tissue, including cortical neurons, bear the brunt of oxygen shortage because they depend on oxygen to continuously produce metabolic energy [[49]4,[50]7,[51]15]. Neuron death is an apparent pathological change in the ischemia cortical region [[52]16]; therefore, further studies should examine how cortical neurons perceive oxygen and identify the adaptive systems that cortical neurons use to cope with hypoxia. Omics approaches are powerful tools for clarifying pathogenic mechanisms. Previous studies have shown that hypoxia induces adaptive changes in many cellular events, including metabolic adaptations [[53]16,[54]17]. Moreover, metabolites were identified as regulators or indicators in ischemic reperfusion and other hypoxia-associated conditions [[55][18], [56][19], [57][20], [58][21], [59][22]]. Single omics (e.g., microarray and transcriptomics) approaches enable us to dissect the underlying mechanisms of cellular adaptations under hypoxic conditions [[60]23]. Yet, despite considerable advances in our understanding of cellular adaptations to hypoxia promoted by single omics, a more detailed assessment of the hypoxic response, particularly from an integrative analysis perspective, has not been performed yet. Multi-omics analysis provides insights into pathogenic mechanisms, allowing us to interrogate diseases from multiple perspectives. Here, we combined metabolic and transcriptomic analysis to probe the molecular basis of acute hypoxia in cortical neurons. Our integrated analysis revealed that hypoxia in primary cortical neurons significantly alters metabolic and hypoxia-inducible factor 1 (HIF-1) transcriptional signaling pathways. Therefore, targeting these pathways is a potential therapeutic option for treating hypoxia-related ischemic shock and other diseases. 2. Materials and methods 2.1. Chemicals As previously described [[61]24], all chemicals and solvent reagents used were HPLC or analytical grade. 2.2. Primary cortical neurons culture and hypoxia treatment Primary cortical neurons (PCNs) were cultured as previously described [[62]25,[63]26]. The PCNs cultures were maintained for 11 days in vitro (DIV) and incubated in a hypoxia chamber (Smartor 118pro, Hua Yue Enterprise Holdings Ltd., Guangzhou, China) containing 0.1% Oxygen/5%CO2/94.9N2) for 2 h. Then, cells were collected for subsequent mRNA extraction (n = 3), RNA-sequencing (RNA-seq) (n = 3), and metabolomics analysis (n = 6). The protocol used to prepare primary cortical neuron cultures from mice was approved by the research ethics committee of the Tongren Hospital, Shanghai Jiao Tong University School of Medicine. 2.3. Apoptosis detection by TUNEL assay PCNs subjected to normoxia or acute hypoxia were fixed with 4% paraformaldehyde, and the apoptotic cells were detected using the One-step TUNEL Apoptosis Assay kit (#C1090, Shanghai, China). Prior to mounting, the cells were counterstained with the nuclear dye Hoechst33342 (DOJINDO, Japan). The apoptosis rate was calculated as the number of TUNEL-positive cells divided by the number of Hoechst33342-stained cells. Images were acquired under an A1-scope fluorescence microscopy (Zeiss, Germany). 2.4. RNA isolation and RNA-seq library construction The RNA extraction and sequencing library construction were performed as previously described [[64]24]. 2.5. RNA-seq and differentially expressed genes (DEGs) analysis An Illumina NovaSeq 5000 platform sequenced the RNA libraries and generated 150 bp paired-end reads. The raw reads ([65]BioProject accession number PRJNA827649) were technically processed as previously described [[66]24], and then gene expression was analyzed using the DESeq (2012) R package [[67]27]. A p-value <0.05 and an |FC| >1.2 were applied to screen for DEGs and shown by hierarchical cluster analysis. Then the DEGs were used in the Kyoto encyclopedia of genes and genomes (KEGG) [[68]28] pathway enrichment analysis with OEcloud ([69]https://cloud.oebiotech.com/task/). Gene ontology (GO) enrichment was performed in Metscape ([70]https://metascape.org/gp/index.html). Gene set enrichment analysis (GSEA) was employed to screen for pathways related to biological events, using the following cut-offs: KEGG pathway terms with enrichment score (ES) > 0.40, normalized enrichment score (NES) > 1.4, and p < 0.01 were considered significantly enriched. 2.6. Reverse transcription-quantitative polymerase chain reaction (RT-qPCR) RNA extraction and RT-qPCR were performed as previously described [[71]24,[72]25,[73]29]. All primers used in validated genes are listed in [74]Supplementary Table 1. 2.7. Non-targeting metabolomics analysis As reported in our recent studies [[75]24,[76]30], we performed LC-MS-based metabolomics analysis using the OE Biotechnology Co. Ltd (Shanghai, China) platform. Briefly, ∼1 × 10^7 11-DIV cultured PCNs in acute hypoxia or normoxia (n = 6) were used to prepare LC-MS samples by sonication with chloroform and dissociation with methanol: water (1:4) solution. Subsequently, these samples were separated by ultra-performance liquid chromatography (UPLC) on a Nexera UPLC System (Shimadzu Corporation, Japan). Then, a Q Exactive mass spectrometer was employed to acquire MS/MS spectra with information-dependent acquisition (IDA) mode under the Xcalibur 4.0.27 software (Thermo Fisher). Lastly, the acquired LC-MS raw data were processed in Progenesis QI v2.3 (Waters Corporation, Milford, USA) to identify metabolites based on public databases, including the human metabolome database (HMDB) ([77]http://www.hmdb.ca/), METLIN and Lipid Maps (v2.3) ([78]http://www.lipidmaps.org/). The resulting metabolites were further analyzed by the principal component analysis (PCA) and the orthogonal projections to latent structures discriminant analysis (OPLS-DA) to determine metabolic alterations in the hypoxia (H) and normoxia (N) groups. The criteria for differentially expressed metabolites (DEMs) were variable importance in the projection (VIP) > 1.0 as determined by OPLS-DA) and p < 0.05, as shown by a two-tailed Student's t-test on the normalized peak areas. 2.8. Integrated pathway analysis DEGs ( [MATH: |FC| :MATH] >1.2, p < 0.05) and DEMs (VIP>1, p < 0.05) were used for integrated analysis by Metabolyst 5.0 [[79]31]. We selected all pathway (integrated) databases, the hypergeometric test enrichment, and the combined p-values (pathway-level) integration method to compare results from integrated pathway analysis. 2.9. Statistical analysis The raw data for each group were statistically analyzed by unpaired Student's t-test tested with GraphPad Prism 8 software. Data represented as mean ± SD. Differences with p < 0.05 were considered significant, and differences with p ≥ 0.05 were considered non-significant. 3. Results 3.1. Acute hypoxia increases vascular endothelial growth factor A (Vegfa) mRNA expression and causes apoptosis in primary cortical neurons We first constructed the hypoxia model with the cultured mouse PCNs, followed by a severe hypoxic treatment (0.1% O[2]) for 2 h. RT-qPCR analysis showed that hypoxia marker Vegfa mRNA increased ∼2.8 fold in the hypoxia group when compared to the normoxia group ([80]Fig. 1A), in line with previous studies [[81]32,[82]33]. In addition, acute hypoxia led to cortical neuron apoptosis, in contrast to normoxia ([83]Fig. 1B and C). These results indicated that our model of primary cortical neurons reflected the hallmarks of hypoxia and therefore could be used for subsequent studies. Fig. 1. [84]Fig. 1 [85]Open in a new tab Acute hypoxia increases Vegfa mRNA expression and causes apoptosis of primary cortical neurons. (A) Vegfa mRNA upregulated in primary cortical neurons undergoing acute severe hypoxia. Cultured mouse cortical neurons (11-DIV) were incubated in a hypoxia chamber containing 0.1% O[2] for 2 h and collected for Vegfa and Hif1a RT-qPCR analysis. Mean ± SD, n = 4, unpaired student's t-test, ***p < 0.001, ns, no significant. (B) Representative TUNEL staining of PCNs in Acute hypoxia. Red, Cy3-labeled TUNEL-positive cells; Blue, Hoechst counterstaining. Bar 50 μm. (C) The apoptosis rate in (B) was quantified by calculating the ratio of TUNEL-positive cells to Hoechst-stained cells. Data are expressed as mean ± SD (n = 5–6), unpaired Student's t-test, **p < 0.001. (For interpretation of the references to color in this figure legend, the reader is referred to