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Although superhydrophobic surfaces are developed for analyte enrichment, i.e., to concentrate and transfer analytes toward a specific position, it is still challenging to realize reproducible, uniform, and sensitive superhydrophobic SERS substrates over large scales, representing a major barrier for practical sensing applications. To overcome this challenge, a superhydrophobic SERS chip that combines 3D\u2010assembled gold nanoparticles on nanoporous substrates is proposed, for a strong localized field, with superhydrophobic surface treatment for analyte enrichment. Intriguingly, by concentrating droplets in the volume of 40\u00a0\u00b5L, the sensitivity of 1\u00a0n<jats:sc>m<\/jats:sc> is demonstrated using 1,2\u2010bis(4\u2010pyridyl)\u2010ethylene molecules. In addition, this unique chip demonstrates a relative standard deviation (RSD) of 2.2% in chip\u2010to\u2010chip reproducibility for detection of fentanyl at 1\u00a0\u00b5g\u00a0mL<jats:sup>\u20131<\/jats:sup> concentration, revealing its potential for quantitative sensing of chemicals and drugs. Furthermore, the trace analysis of fentanyl and fentanyl\u2010heroin mixture in human saliva is realized after a simple pretreatment process. This superhydrophobic chip paves the way toward on\u2010site and real\u2010time drug sensing to tackle many societal issues like drug abuse and the opioid crisis.<\/jats:p>","DOI":"10.1002\/smll.202204234","type":"journal-article","created":{"date-parts":[[2022,10,19]],"date-time":"2022-10-19T20:02:20Z","timestamp":1666209740000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":27,"title":["Superhydrophobic 3D\u2010Assembled Metallic Nanoparticles for Trace Chemical Enrichment in SERS Sensing"],"prefix":"10.1002","volume":"18","author":[{"ORCID":"https:\/\/orcid.org\/0000-0003-3639-2643","authenticated-orcid":false,"given":"Youhai","family":"Liu","sequence":"first","affiliation":[{"name":"Department of Electrical Engineering University at Buffalo The State University of New York  Buffalo NY 14260 USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Nan","family":"Zhang","sequence":"additional","affiliation":[{"name":"Department of Electrical Engineering University at Buffalo The State University of New York  Buffalo NY 14260 USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Dylan","family":"Tua","sequence":"additional","affiliation":[{"name":"Department of Electrical Engineering University at Buffalo The State University of New York  Buffalo NY 14260 USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yingkun","family":"Zhu","sequence":"additional","affiliation":[{"name":"Department of Electrical Engineering University at Buffalo The State University of New York  Buffalo NY 14260 USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jacob","family":"Rada","sequence":"additional","affiliation":[{"name":"Department of Electrical Engineering University at Buffalo The State University of New York  Buffalo NY 14260 USA"},{"name":"Material Science Engineering Physical Science and Engineering Division King Abdullah University of Science and Technology  Thuwal 23955\u20136900 Kingdom of Saudi Arabia"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Wenhong","family":"Yang","sequence":"additional","affiliation":[{"name":"Material Science Engineering Physical Science and Engineering Division King Abdullah University of Science and Technology  Thuwal 23955\u20136900 Kingdom of Saudi Arabia"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Haomin","family":"Song","sequence":"additional","affiliation":[{"name":"Department of Electrical Engineering University at Buffalo The State University of New York  Buffalo NY 14260 USA"},{"name":"Material Science Engineering Physical Science and Engineering Division King Abdullah University of Science and Technology  Thuwal 23955\u20136900 Kingdom of Saudi Arabia"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Alexis C.","family":"Thompson","sequence":"additional","affiliation":[{"name":"Department of Psychology University at Buffalo The State University of New York  Buffalo NY 14203 USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"R. 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