Determination of triazines herbicides (atrazine and simazine) by high performance liquid chromatography (HPLC) in samples of trophic chain were worked out. Determination limits of 0.5 μg g −1 for atrazine, 0.8 μg g −1 for simazine with pesticides recovery of 70–77% in trophic chain samples were obtained. The content of simazine in soils was in range 1.72–57.89 μg g −1, in grass 5–88 μg g −1, in milk 2.32–15.29 μg g −1, in cereals 10.98–387 μg g −1, in eggs 30.14–59.48 μg g −1, for fruits: 2.45–6.19 μg g −1. The content of atrazine in soils was in range 0.69–19.59 μg g −1, in grass 7.85–23.85 μg g −1, in cereals 1.88–43.08 μg g −1. Cadmium, lead and zinc were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) in the same samples as atrazine and simazine. Determination limits for cadmium 5 × 10 −3 μg g −1, for lead 1 × 10 −2 μg g −1, and for zinc 0.2 × 10 −3 μg g −1, were obtained. The content of cadmium in soil was in range 0.13–5.89 μg g −1, in grass 114–627.72 × 10 −3 μg g −1, in milk 8.88–61.88 × 10 −3 μg g −1, in cereals 0.20–0.31 μg g −1, in eggs 0.11–0.15 μg g −1, in fruits 0.23–0.59 μg g −1. The content of lead in soils was in range 0.57–151.50 μg g −1, in grass 0.16–136.57 μg g −1, in milk 1.16–3.74 μg g −1, in cereals 1.05–5.47 μg g −1, in eggs 5.79–55.87 μg g −1, in fruits 21.00–87.36 μg g −1. Zinc content in soil was in range 9.15–424.5 μg g −1, in grass 35.20–55.87 μg g −1, in milk 20.00–34.38 μg g −1, in cereals 14.94–28.78 μg g −1, in eggs 15.67–32.01 μg g −1, in fruits 14.94–18.88 μg g −1. Described below extraction and mineralization methods for particular trophic chains allowed to determine of atrazine, simazine, cadmium, lead and zinc with good repeatability and precision. Emphasis was focused on liquid–liquid extraction and solid-phase extraction of atrazine and simazine from analysed materials, as well as, on monitoring the content of herbicides and metals in soil and along trophic chain. Higher concentration of pesticides in samples from west region of Poland in comparison to that of east region is likely related to common applying them in Western Europe in relation to East Europe. The content of metals strongly depends on samples origin (industry area, vicinity of motorways).