To increase the analytical effectiveness of spectrophotometric detection of zinc (Zn(II)) in water, food, tobacco, and pharmaceutical preparations samples, cloud point extraction (CPE) and a new chromogenic reagent were used in this study. The proposed methodology is based on measuring the absorbance of a Zn(II) complex with 2-amino-4-(4-nitrophenyl) diazenyl) pyridine-3-ol (ANPDP) at pH 9.0 in Triton X-114 at maximum 595 and maximum 605 nm for methods without and with CPE. Investigation and optimization were done on the key variables determining CPE effectiveness. For techniques without CPE and with CPE, respectively, the calibration graph was linear under ideal conditions in the ranges of 10-140 µg mL-1 and 0.01-0.8 µg mL-1, with R2 = 0.9989 and 0.9997, respectively. For techniques without CPE and with CPE, the detection limits were 3.0 µg mL-1 and 0.003 µg mL-1 with a preconcentration factor of 50, respectively. As precision, the relative standard deviation (RSD%) is 4.0%. The interactions of various cations and anions have been studied. The proposed CPE method was successfully used to estimate Zn(II) in a variety of samples, including water, food, tobacco, and pharmaceutical preparations.