Senescence and levels of minerals, sugars, and proteins were determined in stalk internodes of corn (Zea mays L.) cv. Illini Gold, a shrunken2 hybrid, from from mid-whorl (V9; internodes completely juvenile) to fresh-market maturity (FM; internodes exhibiting stages of senescence). Senescence was rated in internodes near the base of the stalk (I7), below the ear (I9), and between the ear and tassel (I11). Tissues were extracted and analyzed by carbon-nuclear magnetic resonance spectroscopy (C-nmr) and SDS-PAGE electrophoresis. Senescence rating increased from V9 to FM. Through silk emergence (R1) C-nmr carbohydrate spectra were similar, regardless of internode, with chemical shifts between 61 and 104 ppm, mostly of glucose, fructose, and sucrose. At FM, additional lines were found that were not associated with a saccaride. The highest concentration of sucrose was at R1, fructose at tasseling (VT), and R1, and for glucose from VT to FM. The protein profile present through R1 in I7 was not present at FM. In I9, the protein profile was similar throughout. In I11, numbers, or density, of protein bands decreased through FM. Mineral concentrations did not change, decreased, or fluctuated. Levels of N, Cl, or Na at VT, R1, and FM, respectively, were negatively correlated with senescence. In I7 and I9, senescence ratings were negatively correlated with levels of Mg, NO–3, or SO2–4. Senescence appears to be associated with concentrations of some minerals, a reduction in levels of sucrose, and with the presence or absence of some proteins; however, cause and effect remains to be established. This research was hosted by USDA/SCARL at Lane, Okla., and made use of NMR equipment provided through USAF/AFOSR Grant F49620-95-1-0316 and NIH/NIGMS Grant GM 08003.