Hibiscus Rosa sinensis is a well-recognized medicinal herb for its high phytochemical such as ascorbic acid and phenolic contents. Titration procedure was applied for determine the quantitative amount of ascorbic acid and phenolic content and tries to establish a relationship in both phytochemicals within plant parts such as leaves, stem and flowers. Hibiscus Rosa sinensis plant harvested into three different stages such as leaves, stem and flowers parts extracts. Ascorbic acid and phenolic content in plant parts were evaluated through titration methods and Folin-Ciocalteau reagent methods respectively. The leaves contained 65.48 ± 2.08 mg/100 g, ascorbic acid, stem had 46.98 ± 0.51 mg/100 g and flowers contained were 26.48 ± 1.44 mg/100 g. The phenolic content in leaves, stem and flower extracts were also calculated and found 43.31 ± 0.71 mg, 41.79 ± 1.20 mg and 35.25 ± 1.79 mg of Gallic acid equivalent (GAE) per gram respectively. Five replicates basic data of correlation indicated that the ascorbic acid and phenolic content in leaves, stem and flowers showing a non-significant, negative and positive relationship respectively. The high ascorbic acid contents in leaves showed that they are highly rich in vitamin C and good for the prevention and treatment of vitamin deficiency disease. Phenol content was also observed in higher amount in plant leaves as compare to stem and flowers. It is also observed that the different parts of plants contained different amount of ascorbic acids as well as phenolic content.