Cannabis herbal extracts (CHE) are one of the most interesting and sought products for therapeutic approaches of a diverse number of clinical conditions. Regulated quality control parameters and risk assessment methods are needed for Cannabis-based products. Advanced analytical techniques portray powerful alternatives to Cannabis-based products monitoring. However, further analytical steps need to be critically optimized to keep up with instrumental performance. In this work, analytical methods for phytocannabinoids quantification by UHPLCHRMS/MS and multielement determination by ICP-MS, both in CHE, were developed and optimized by Design of Experiments. For UHPLC-HRMS/MS, an ultrasound-assisted liquid-liquid extraction with methanol:hexane 9:1 v/v was proposed, analytical performance was successfully validated by gold-standard brazilian pharmaceutical guidelines, proving its efficiency in question. For multielement determination, three sample preparation methods were explored (acid decomposition in open-vessel, acid decomposition in closed-vessel, and organic solvent direct dilution). Their performances were critically evaluated regarding analytical metrics, ecological impact and user-friendliness. The open-vessel method with diluted HNO3 provided the overall best performance and was applied to analyze 6 CHEs and one sesame oil sample. The phytocannabinoids quantification suggested a major discrepancy between CHE label description and quantified content, as CBD was over 10,000-times lower and both THC and CBN could not be determined. Also, in general, low metal and metalloid contents were determined, but significant potentially toxic metals content was found. By comparing with sesame oil, statistically significant differences were identified only for Au, Cu, K, Li, Mg, Mn, Ni, Pb, Ti, and Zn. Lead were found at higher levels for all Cannabis samples in a range 11.7 to 12.4 (micro)g g-1 , in disagreement with FDA guidelines for potentially toxic elements (10 (micro)g g-1 ). Li, Mg, Mn, Ni, Ti and Zn were found at discordant levels between samples, suggesting a relevant heterogeneity and non- standardized quality control for these products.