Hawthorn (Crataegus spp.), belonging to the Rosaceae family, is rich in sugars, minerals, and vitamins A and C. The fruits and flowers of many hawthorn varieties are well known as a heart tonic, have hypotensive effects, and are considered to be generally safe and well tolerated [1]. Previous investigations indicate that Chinese Crataegus extracts have beneficial effects, e.g., anti-inflammatory [2], hypolipidemic [3], and antioxidant [4]. Other proprieties have also been elucidated such as anticarcinogenic [5] and antimicrobial [6]. In France, hawthorn is prescribed and marketed in pharmacies as gelatin capsules or as a sedative tea to treat nervosity and sleep disorders [7,8]. The pharmacological effects, including the antioxidant power of Crataegus, have mainly been attributed to polyphenolic compounds like flavonoids and phenolic acids. Currently, investigations on important bioactive and antioxidant phytochemicals in medicinal plants and herbal food materials have received great attention. The aim of the present work was, on the one hand, to highlight the volatile constituents of leaves and flowers of C. azarolus and, on the other hand, to evaluate the antioxidant property of the crude extract. Available information indicates that the essential oil of C. azarolus has not been studied to date. Essential oil extractions were performed using two different processes, initially by the relatively recent method of hydrodistillation assisted by microwave heating (HD-MW), afterwards by hydrodistillation (HD), the conventional technique recommended by AFNOR in the extraction of essential oils destined for the food and cosmetic industries. Many experiments have been performed in this study in order to optimize the yield of the (HD-MW) extract by studying: (a) the extraction time; (b) the radiation power of the microwave oven; (c) the used quantity of water, starting from a dried distillation, as stated in our previous investigations [9,10]. The extracts were analyzed by gas chromatography GC-FID and gas chromatography coupled to mass spectrometry GC-MS. The findings in terms of yield, extraction time, volatile profiling, and quality of the essential oil were compared.Regarding the assessment of the total antioxidant capacity of C. azarolus, we have estimated primarily the total phenolic and flavonoid contents in a methanolic crude extract, molecules to which the antioxidant property is related. Subsequently, two different methods have been used to evaluate this activity, namely the DPPH radical scavenging assay and the E-carotene bleaching test. Descriptive statistical analysis, analysis of correlation coefficients, and one-way analysis of variance were performed.Extraction Yield. The extraction yield was calculated from dry plant material after determining the sample moisture content (54%). An extraction time of 30 min with HD-MW provides yields 0.024 r 0.001% (w/w) slightly higher than HD yields 0.019 r 0.001% (w/w) obtained after 3 h.