ABSTRAK Kulit buah kakao (Theobroma cacao L) telah diisolasi dan diuji aktivitas toksisitasnya dengan menggunakan metode Brine Shrimp Lethality Test (BSLT). Kulit buah Theobroma cacao sebanyak 4 Kg dimaserasi menggunakan pelarut metanol, kemudian dipartisi dengan n-heksana dan diekstraksi dengan etil asetat sehingga diperoleh ekstrak n-heksana, etil asetat dan metanol berturut-turut sebanyak 26,62 g (67,01 %), 0,45 g (1,22 %), 6,61 g (17,99 %). Uji fitokimia ekstrak n-heksana mengandung terpenoid dan steroid, ekstrak etil asetat mengandung alkaloid, flavonoid, steroid dan fenolik, sedangkan ekstrak metanol mengandung alkaloid, flavonoid, saponin, dan fenolik. Uji aktivitas toksisitas ekstrak n-heksana, etil asetat dan metanol diperoleh nilai LC50 berturut-turut yaitu 192,75 ppm, 263,02 ppm dan 79,98 ppm. Ekstrak metanol dilakukan kromatografi kolom gravitasi dan diperoleh 5 fraksi gabungan yaitu Theobroma cacao metanol (TCM 1 - TCM 5). Uji toksisitas dilakukan kembali untuk 5 fraksi gabungan dan diperoleh nilai LC50 berturut-turut yaitu 42,90 ppm, 38,68 ppm, 70,97 ppm, 88,59 ppm dan 62,06 ppm. TCM 2 dilakukan rekromatografi kolom gravitasi dan diperoleh 4 fraksi gabungan yaitu (TCM 2.1 - TCM 2.4) serta dilakukan uji aktivitas toksisitas dengan nilai LC50 berturut-turut yaitu 28,85 ppm, 39,37 ppm, 33,45 ppm dan 63,66 ppm. TCM 2.1 dimurnikan dengan menggunakan KLT preparatif dan diperoleh isolasi murni berwarna merah muda yaitu golongan senyawa terpenoid. Kata Kunci : Kulit Buah Kakao (Theobroma cacao), Ekstrak Metanol, Toksisitas, Brine Shrimp Lethality Test (BSLT) v ABSTRACT Cacao pod husk (Theobroma cacao L) has been isolated and toxicity test using Brine Shrimp Lethality Test (BSLT) method. Theobroma cacao pod husk (4 kg) was macerated using methanol solvent, then partitioned with n-hexane and ethyl acetate to obtain 26,62 g (67.01 %) n-hexane, 0,45 g (1,22%) ethyl acetate and 6,61 g (17,99 %) methanol extract. Phytochemical test of n-hexane extract contains terpenoids and steroids, ethyl acetate extract contains alkaloids, phalvanoids, steroids and phenolics and methanol extract contains alkaloids, flavonoids, saponins, and phenolics. LC50 values of toxicity n-hexane, ethyl acetate and methanol extracts were 192,75 ppm, 263,02 ppm and 79,98 ppm, respectively. Methanol extract was fractionated by gravity column chromatography and obtained 5 combined fractions, they are Theobroma cacao methanol 1 (TCM 1 - TCM 5). The Toxicity was tested for 5 combined fractions and LC50 values were 42,90 ppm, 38,68 ppm, 70,97 ppm, 88,59 ppm and 62,06 ppm respectively. TCM 2 was fractionated by gravity column and obtained 4 combined fractions namely (TCM 2.1 - TCM 2.4). The LC50 values of toxicity (TCM 2.1 -TCM 2.4) were 28,85 ppm, 39,37 ppm, 33,45 ppm and 63,66 ppm respectively. TCM 2.1 was purified using preparative TLC and obtained a single pink compound which is a class of terpenoid compounds. Keyword : Cacao pod husk (Theobroma cacao), Methanol Extract, Toxicity, Brine Shrimp Lethality Test (BSLT).