We have investigated the chloroform extract of a commercially available herbal drug Maydis stigma (dried cut stigmata of maize, Zea mays L. ssp. mays, Poaceae), purchased from the herbal apothecary of the Institute for Medicinal Plant Research "Dr. Josif Pancic", Belgrade, Serbia and Montenegro. Powdered plant material (1.5 kg) was extracted with CHCl3 in a Soxhlet apparatus until exhausted. Dry CHCl3 extract (15 g) was fractionated by silicagel flash CC, using an n-hexane to n-hexaneacetone (50:50, v/v) gradient with 1% rate, followed by an n-hexane–acetone (50:50, v/v) to MeOH gradient with 5% increase. Final elution: MeOH. Fractions with similar composition (monitored by TLC) were pooled together. Compound 1 (200 mg) was isolated from fraction 12 by recrystallization from petroleum ether at +4°C. Compound 2 (1600 mg) was isolated from pooled fractions 24–27 by recrystallization from acetone at +4°C. Compound 3 (50 mg) was isolated from pooled fractions 28–56 by LPLC on Lobar Fertigsaule Grosse B (310–25) LiChroprep Si 60 (40–63 mm) fur die Flussigkeits-Chromatographie (Merck, Darmstadt, Germany) and ChemCo Low-Prep Pump, Model 81-M-2 (ChemCo, Japan), using toluene–ethyl acetate gradient, at a flow rate of 1 ml/min. Compound 4 (500 mg) was isolated from pooled fractions 170–194 by recrystallization from acetone at +4°C. Compound 1 (white, amorphous flakes). Mass spectrum (EI, 70 eV), m/z (Irel, %): 396 [M]+ (6), 382 [M]+ 14 (8), 368 (28), 354 (9), 340 (11), 326 (6), 312 (4), 298 (3), 60 (45, basal ion), 45 (100). 1 was identified as hexacosanoic acid. This compound was isolated from M. stigma for the first time. Compound 2 (colorless prismatic crystals). Mass spectrum (EI, 70 eV), m/z (Irel, %): 414 [M]+ (67), 399 [M]+-Me (27), 396 [M]-H2O (34), 381 [M]+ –Me–H2O (24), 329 (27), 303 (35), 273 (27), 255 (46), 231 (24), 213 (40), 145 (47), and m/z (Irel, %): 412 [M]+ (39), 300 (21), 271 (27), 253 (8), 229 (18), 211 (5). PMR (250 MHz, CDCl3, δ, ppm, J, Hz): 0.6–1.0 (s, CH3-18, 19, 21, 26, 27 and 29, J = 6–7), 3.53 (m, H-3a), 5.33 (d, H-6), 5.12 (dd, H-22), 5.00 (dd, H-23). According to previously published spectral data [1–3], 2 was identified as a mixture of sitosterol and stigmasterol (4:1 ratio). Compound 3 (colorless semisolid). PMR (250 MHz, CDCl3, δ, ppm): 3.48 (1H, s, OH), 2.44 (2H, s, aliphatic CH2), 1.99 (3H, s, CH3), 1.05 (6H, s, 2CH3). 13C NMR (90 MHz, CDCl3, d): 210.5 (C=O), 69.2 (tert-C–OH), 53.7 (aliphatic CH2), 31.4 (CH3 at C=O), 28.9 (2CH3). The presented spectral data are in good agreement with published data on 4-hydroxy-4methyl-2-pentanone [4]. To the best of our knowledge, 3 was isolated from M. stigma for the first time. Compound 4 (white, amorphous solid). The PMR spectra (250 MHz, CDCl3, δ, ppm) are similar to 2, except: 4.91 (1H, d, anomeric H-1′ of glucose), 4.20 (1H, d, H-3′), 4.43 (1 H, t, H-4′), 4.86–4.87 (1H, dd, H-6′). The presented data are consistent with previously published data on daucosterol (β-sitosteryl-3-O-β-D-glucoside, sitosteroline) [3].