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The developed method includes on\u2010target enrichment and detection of phosphopeptides\/phospholipids using graphene oxide\u2013lanthanide metal oxides (samarium, gadolinium, dysprosium, and erbium) nanocomposites. Enriched phosphopeptides are detected using material enhanced laser desorption\/ionization mass spectrometry and phospholipids by laser desorption\/ionization\u2010mass spectrometry. Nanocomposites are prepared using graphene oxide with respective metal salts at high pH. They are characterized for nano\u2010morphology, chemistry, porosity, composition, crystallinity, and thermal stability. Phosphopeptides enrichment protocol is developed and optimized for tryptic \u03b2\u2010casein digest and that of phospholipids by phosphatidylcholine standard. Statistical analyses of phosphopeptides and phospholipids from milk show overlapping results for gadolinium, dysprosium, and erbium oxide nanocomposites. GO\u2010Gd<jats:sub>2<\/jats:sub>O<jats:sub>3<\/jats:sub> has better enrichment efficiency and application as LDI material. Selectivity for GO\u2010Dy<jats:sub>2<\/jats:sub>O<jats:sub>3<\/jats:sub> is 1:2500, for GO\u2010Sm<jats:sub>2<\/jats:sub>O<jats:sub>3<\/jats:sub> is 1:3500, and 1:4000 for GO\u2010Gd<jats:sub>2<\/jats:sub>O<jats:sub>3<\/jats:sub>. GO\u2010Er<jats:sub>2<\/jats:sub>O<jats:sub>3<\/jats:sub> has a sensitivity of 25 fmol, whereas the highest sensitivity is down to 0.5 fmol for GO\u2010Gd<jats:sub>2<\/jats:sub>O<jats:sub>3<\/jats:sub>. On\u2010target enrichment is batch to batch reproducible with a standard deviation of\u00a0&lt;1, reduced time of enrichment to 10\u00a0min, and ease of operation compared to solid\u2010phase batch extraction. The developed method enriches serum phosphopeptides characteristic of cancer\u2010related phosphoproteins.<\/jats:p>","DOI":"10.1002\/jssc.202001276","type":"journal-article","created":{"date-parts":[[2021,6,24]],"date-time":"2021-06-24T09:00:25Z","timestamp":1624525225000},"page":"3137-3145","update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":11,"title":["Graphene oxide\u2013metal oxide nanocomposites for on\u2010target enrichment and analysis of phosphorylated biomolecules"],"prefix":"10.1002","volume":"44","author":[{"given":"Fahmida","family":"Jabeen","sequence":"first","affiliation":[{"name":"Division of Analytical Chemistry Institute of Chemical Sciences Bahauddin Zakariya University  Multan Pakistan"},{"name":"Department of Chemistry The Women University  Multan Pakistan"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Muhammad Salman","family":"Sajid","sequence":"additional","affiliation":[{"name":"Division 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