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Zn\u2010MOF is used as a template for MoS<jats:sub>2<\/jats:sub> nanosheets synthesis and further carbonized to yield light\u2010responsive ZnS\/C\/MoS<jats:sub>2<\/jats:sub> nanocomposites. Zn\u2010MOF, carbonized\u2010Zn\u2010MOF, and ZnS\/C\/MoS<jats:sub>2<\/jats:sub> nanocomposites are characterized by Fourier transform infrared spectroscopy, transmission electron microscopy, X\u2010ray diffraction pattern, scanning electron microscopy (SEM), element mapping, Raman spectroscopy, X\u2010ray photoelectron spectroscopy, fluorescence, and nitrogen\u2010adsorption analysis. Carcinoembryonic antigen (CEA) is selected as a model to construct an immunosensing platform to evaluate the photo\u2010electrochemical (PEC) performances of ZnS\/C\/MoS<jats:sub>2<\/jats:sub> nanocomposites. A sandwich\u2010type PEC immunosensor is fabricated by immobilizing CEA antibody (Ab<jats:sub>1<\/jats:sub>) onto the ZnS\/C\/MoS<jats:sub>2<\/jats:sub>\/GCE surface, subsequently binding CEA and the alkaline phosphatase\u2010gold nanoparticle labeled CEA antibody (ALP\u2010Au\u2010Ab<jats:sub>2<\/jats:sub>). The catalytic conversion of vitamin C magnesium phosphate produces ascorbic acid (AA). Upon being illuminated, AA can react with photogenerated holes from ZnS\/C\/MoS<jats:sub>2<\/jats:sub> nanocomposites to generate a photocurrent for quantitative assay. Under optimized experimental conditions, the PEC immunosensor exhibits excellent analytical characteristics with a linear range from 2.0 pg mL<jats:sup>\u22121<\/jats:sup> to 10.0 ng mL<jats:sup>\u22121<\/jats:sup> and a detection limit of 1.30 pg mL<jats:sup>\u22121<\/jats:sup> (S\/N = 3). The outstanding practicability of this PEC immunosensor is demonstrated by accurate assaying of CEA in clinical serum samples.<\/jats:p>","DOI":"10.1002\/smll.201902086","type":"journal-article","created":{"date-parts":[[2019,7,30]],"date-time":"2019-07-30T12:19:51Z","timestamp":1564489191000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":45,"title":["ZnS\/C\/MoS<sub>2<\/sub> Nanocomposite Derived from Metal\u2013Organic Framework for High\u2010Performance Photo\u2010Electrochemical Immunosensing of Carcinoembryonic Antigen"],"prefix":"10.1002","volume":"15","author":[{"given":"Qiuxi","family":"Wei","sequence":"first","affiliation":[{"name":"Key Laboratory of Analytical Chemistry of the State Ethnic Affairs Commission College of Chemistry and Materials Science South\u2010Central University for Nationalities  Wuhan 430074 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