Concentrations and secretion rates of macronutrients and major ions in human milk during lactogenesis (birth to 8 d) and late lactation (greater than 6 mo postpartum) are reported. Postpartum changes in lactose, sodium, and chloride concentrations signalled closure of the paracellular pathway during days 1-2. From days 2 to 4 postpartum, initiation of copious milk secretion was accompanied by significant increases in citrate, free phosphate, glucose, and calcium concentrations and a decrease in pH. During weaning, significant changes in milk protein, lactose, chloride, and sodium concentrations were observed only when milk volume fell below 400 mL/d; more than one feed per day was necessary to maintain milk secretion. Temporal changes in the concentration of other milk components, except glucose and magnesium, were not different in weaning and non-weaning women. Differences between the relation of milk volume and composition during lactogenesis and weaning suggest that volume is differently regulated in the two periods.