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Caseinomacropeptide (CMP) is released from bovine kappa-casein after rennet treatment and is one of the major peptides in whey protein isolate. CMP has in vitro anti-inflammatory and antibacterial activities. CMP has two major amino acid sequences with different modifications, including glycosylation, phosphorylation and oxidation. However, no previous work has provided a comprehensive profile of intact CMP. Full characterization of CMP composition and structure is essential to understand the bioactivity of CMP. In this study, we developed a top-down glycopeptidomics-based analytical method to profile CMP and CMP-derived peptides using Orbitrap mass spectrometry combined with nano-liquid chromatography with electron-transfer/higher-energy collision dissociation. The liquid chromatography–tandem mass spectrometry (LC–MS/MS) spectra of CMPs were annotated to confirm peptide sequence, glycan composition and other post-translational modifications using automatic data processing. Fifty-one intact CMPs and 159 CMP-derived peptides were identified in four samples (one CMP standard, two commercial CMP products and one whey protein isolate). Overall, this novel approach provides comprehensive characterization of CMP and CMP-derived peptides and glycopeptides, and it can be applied in future studies of product quality, digestive survival and bioactivity.

Pectin is a co-product from juicing and the physico-chemical quality is important to functionality of pectin in food and pharmaceutical applications. Juice and peel from Huanglongbing (HLB) control and infected Valencia oranges were analyzed. Infected fruit had smaller diameter, lower L* and b* values and highly variable a* values. Juice from infected fruit had higher pectinmethylesterase (PME) activity of 1.5 Units/mL, which retained higher activity during 15 days of storage at 4 °C, and juice had higher cloud loss. Also, the juice obtained from infected fruit had lower °Brix (8.5–8.9), higher titratable acidity (0.71–0.88%), and lower pH (3.45–3.75). Molecular weights of 154–157 kDa and degrees of esterification of 65–67% were similar. Pectin yield from dried peel was reduced by 6% in infected fruit to 4.18 g/100 g. Total neutral sugars in pectin from control fruit were higher, 84.1 μg/mg, compared to infected fruit, 60.7 μg/mg. Glucose, galactose, and arabinose, were higher in control fruit, 25.0, 40.8, and 9.7 μg/mg, compared to 14.5, 27.4, and 8.3 μg/mg in infected fruit. Viscosity was 0.015 Pa s, in 1% pectin from control or infected fruit (p > 0.05). Juice quality, including cloud stability, was negatively impacted by HLB, however pectin functionality was minimally impacted.

Pectins from highbush blueberry powder were sequentially solubilized in water, chelator, and sodium carbonate solvents and precipitated (ADF.WSF, ADF.CSF, and ADF.NSF) or not precipitated in ethanol (DF.WSF, DF.CSF, and DF.NSF) before dialysis and freeze-drying. Alcohol precipitation more effectively removed bound anthocyanins and low molar mass pectins from water- and chelator soluble fractions than dialysis alone. Blueberry water soluble fractions were high methoxyl pectins, rich in neutral sugars (36 to 38 mol%), and had high molar mass (7.01 × 105 to 2.71 × 106 g/mol). Blueberry chelator soluble fractions were low methoxyl pectins and rich in uronic acids (90 to 92 mol%) which were more linear and less branched structure than other fractions or commercial citrus pectin. The molar mass ranged from 1.59 × 106 to 2.06 × 106 g/mol. Water- and chelator soluble fractions exhibited pseudoplastic behavior (n