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Most cases of HCC develop in patients that already have liver cirrhosis and have been recommended for surveillance for an early onset of HCC. Cirrhosis is the final common pathway for several etiologies of liver disease, including hepatitis B and C, alcohol, and increasingly non\u2010alcoholic fatty liver disease. Only 20\u201330% of patients with HCC are eligible for curative therapy due primarily to inadequate early\u2010detection strategies. Reliable, accurate biomarkers for HCC early detection provide the highest likelihood of curative therapy and survival; however, current early\u2010detection methods that use abdominal ultrasound and serum alpha fetoprotein are inadequate due to poor adherence and limited sensitivity and specificity. There is an urgent need for convenient and highly accurate validated biomarkers for HCC early detection. The theme of this review is the development of new methods to discover glycoprotein\u2010based markers for detection of HCC with mass spectrometry approaches. We outline the non\u2010mass spectrometry based methods that have been used to discover HCC markers including immunoassays, capillary electrophoresis, 2\u2010D gel electrophoresis, and lectin\u2010FLISA assays. We describe the development and results of mass spectrometry\u2010based assays for glycan screening based on either MALDI\u2010MS or ESI analysis. These analyses might be based on the glycan content of serum or on glycan screening for target molecules from serum. We describe some of the specific markers that have been developed as a result, including for proteins such as Haptoglobin, Hemopexin, Kininogen, and others. We discuss the potential role for other technologies, including PGC chromatography and ion mobility, to separate isoforms of glycan markers. Analyses of glycopeptides based on new technologies and innovative softwares are described and also their potential role in discovery of markers of HCC. These technologies include new fragmentation methods such as EThcD and stepped HCD, which can identify large numbers of glycopeptide structures from serum. The key role of lectin extraction in various assays for intact glycopeptides or their truncated versions is also described, where various core\u2010fucosylated and hyperfucosylated glycopeptides have been identified as potential markers of HCC. Finally, we describe the role of LC\u2010MRMs or lectin\u2010FLISA MRMs as a means to validate these glycoprotein markers from patient samples. 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