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Abstract Surface‐enhanced Raman scattering (SERS) sensing in microfluidic devices, namely optofluidic‐SERS, suffers an intrinsic tradeoff between mass transport and hot spot density, both of which are required for ultrasensitive detection. To overcome this compromise, photonic crystal‐enhanced plasmonic mesocapsules are synthesized, utilizing diatom biosilica decorated with in‐situ growth silver nanoparticles (Ag NPs). In the optofluidic‐SERS testing of this study, 100× higher enhancement factors and more than 1,000× better detection limit are achieved compared with traditional colloidal Ag NPs, the improvement of which is attributed to unique properties of the mesocapsules. First, the porous diatom biosilica frustules serve as carrier capsules for high density Ag NPs that form high density plasmonic hot‐spots. Second, the submicron‐pores embedded in the frustule walls not only create a large surface‐to‐volume ratio allowing for effective analyte capture, but also enhance the local optical field through the photonic crystal effect. Last, the mesocapsules provide effective mixing with analytes as they are flowing inside the microfluidic channel. The reported mesocapsules achieve single molecule detection of Rhodamine 6G in microfluidic devices and are further utilized to detect 1 × 10⁻⁹mof benzene and chlorobenzene compounds in tap water with near real‐time response, which successfully overcomes the constraint of traditional optofluidic sensing. 

Detection of illicit drug residues from wastewater provides a new route toward community-level assessment of drug abuse that is critical to public health. However, traditional chemistry analytical tools such as high-performance liquid chromatography in tandem with mass spectrometry (HPLC-MS) cannot meet the large-scale testing requirement in terms of cost, promptness, and convenience of use. In this article, we demonstrated ultra-sensitive and portable surface-enhanced Raman scattering sensing (SERS) of fentanyl, a synthetic opioid, from sewage water and achieved quantitative analysis through principal component analysis and partial least-squares regression. The SERS substrates adopted in this application were synthesized by in situ growth of silver nanoparticles on diatomaceous earth films, which show ultra-high sensitivity down to 10 parts per trillion in artificially contaminated tap water in the lab using a commercial portable Raman spectrometer. Based on training data from artificially contaminated tap water, we predicted the fentanyl concentration in the sewage water from a wastewater treatment plant to be 0.8 parts per billion (ppb). As a comparison, the HPLC-MS confirmed the fentanyl concentration was below 1 ppb but failed to provide a specific value of the concentration since the concentration was too low. In addition, we further proved the validity of our SERS sensing technique by comparing SERS results from multiple sewage water treatment plants, and the results are consistent with the public health data from our local health authority. Such SERS sensing technique with ultra-high sensitivity down to sub-ppb level proved its feasibility for point-of-care detection of illicit drugs from sewage water, which is crucial to assess public health.