Chrysin, a naturally occurring flavone, extracted from traditional Chinese herbs and abundantly found in propolis has been known to exhibit a wide range of biological activities, such as antioxidant, anti-inflammatory, hypolipidemic, anti-hypertensive, anti-diabetic, and anti-tumour activities. Among this, its anticancer effects make chrysin promising to be a candidate drug. The objective of this study was to develop a new certified reference material (CRM) for the quality control of traditional Chinese medicine, chrysin, and the related pharmaceuticals. The studies of sample preparation, homogeneity, stability, value assignment, and uncertainty evaluation were accomplished in this paper. Two different methods, namely differential scanning calorimetry and coulometric titration, were utilized for the first time to determine the purity of chrysin. The purity of the highpurity chrysin CRM, after validation and evaluation, was certified to be (0.996 ± 0.015) g/g (k = 2).