The main goal of this work was to measure the total alkaloid content (TALC) from pulp, peel, seed, and columella of soursop fruit (Annona muricata L.) by ultrasound-assisted extraction (UAE) and to obtain the best conditions of the UAE with the response surface methodology (RSM). We evaluated the effect of amplitude (40%, 70%, and 100%), time (5, 10, and 15 min) and pulse-cycles (0.4, 0.7, and 1 s) and compared the best UAE conditions of alkaloids with a conventional extraction (maceration). The structural characterization of the raw material with the highest TALC was developed using nuclear magnetic resonance (NMR) techniques [¹H, ¹³C, heteronuclear single quantum correlation (HSQC), heteronuclear multiple bond correlation (HMBC), and homonuclear correlation spectroscopy (COSY)]. According to the RSM, the best conditions in the UAE for extracting alkaloids varied depending on the type of plant tissue. It took 5 min with an amplitude of 70% and pulse-cycles of 1, 0.4, and 1 s, respectively, to extract the highest TALC in peel, seed, and columella while the optimal conditions for extracting the largest amount of alkaloids from the pulp were obtained at 5 min in UAE with pulse-cycles of 0.55 s and 100% amplitude. The TALC was highest in the peel (7.48 mg/g), which was followed by the seed (2.31 mg/g), the pulp (1.20 mg/g), and the columella (0.79 mg/g) and was positively correlated (R² = 0.98–0.88) with the predicted values. In addition, the extraction alkaloids from the peel, pulp, seed, and columella using the UAE was 56.31, 5.45, 3.06, and 2.96 times higher, respectively, than the extraction by maceration. The alkaloids identified in the peel have not been reported and were nornuciferin, assimilobin, anonaine, and isolaureline. This study showed that the soursop fruit peel can be a source of alkaloids and that UAE has an important potential for extracting these compounds.

Collagen hydrolysates are dietary supplements used for nutritional and medical purposes. They are complex mixtures of low‐molecular‐weight peptides obtained from the enzymatic hydrolysis of collagen, which provide intrinsic batch‐to‐batch heterogeneity. In consequence, the quality of these products, which is related to the reproducibility of their mass distribution pattern, should be addressed. Here, we propose an analytical approach to determine the peptide pattern as a quality attribute of Colagenart®, a product containing collagen hydrolysate. In addition, we evaluated the safety by measuring the viability of two cell lines exposed to the product. The consistency of peptide distribution was determined using Size Exclusion Chromatography (SEC), Mass Spectrometry coupled to a reversed phase UPLC system (MS‐RP‐UPLC), and Shaped‐pulse off‐resonance water‐presaturation proton nuclear magnetic resonance spectrometry [ ¹ Hwater_presat NMR]. The mass distribution pattern determined by SEC was in a range from 1.35 to 17 kDa, and from 2 to 14 kDa by MS‐RP‐UPLC. [ ¹ Hwater_presat NMR] showed the detailed spin‐systems of the collagen hydrolysates components by global assignment of backbone Hα and NH, as well as side‐chain proton resonances. Additionally, short‐range intraresidue connectivity pathways of identified spin‐regions were obtained by a 2D homonuclear shift correlation Shaped‐pulse solvent suppression COSY scheme. Safety analysis of Colagenart® was evaluated in CaCo‐2 and HepG2 cells at 2.5 and 25 μg/mL and no negative effects were observed. The results demonstrated batch‐to‐batch reproducibility, which evinces the utility of this approach to establish the consistency of the quality attributes of collagen hydrolysates. Practical Application: We propose state‐of‐the art analytical methodologies (SEC, MS, and NMR) to evaluate peptide profile and composition of collagen hydrolysates as quality attributes. These methodologies are suitable to be implemented for quality control purposes.

A choline chloride/urea natural deep eutectic solvent (ChCl NADES) was prepared via a green chemistry method and used to leach Zn and Mn oxides from conventional Zn–C scrap batteries. FTIR and ¹H NMR spectroscopy were used to characterize the NADES. The leaching kinetics of the Zn and Mn oxides was monitored at isothermal conditions (80, 100, 125, and 150 °C) and at two solid/NADES ratios: 3.3 and 10 g dm⁻³. It was possible to dissolve Zn and Mn oxides under all of tested conditions, reaching more than a 95% recovery for both metals at 150 °C after 90 min, whereas, at 25 °C, it was possible to leach up to 90% of the Zn and 30% of the Mn after 4320 min (72 h). Furthermore, the leaching kinetics was controlled by the boundary layer, coincident with a shrinking core model. According to the Arrhenius plot, the activation energy for Zn ranges from 49.13 to 52.21 kJ mol⁻¹, and that for Mn ranges from 46.97 to 66.77 kJ mol⁻¹.