Oxidation of imidacloprid insecticide through PMS activation using CuFe2O4 nanoparticles: Role of process parameters and surface modifications.

The contamination of water bodies by synthetic organic compounds coupled with climate change and the growing demand for water supply calls for new approaches to water management and treatment. To tackle the decontamination issue, the activation of peroxymonosulfate (PMS) using copper magnetic ferrite (CuMF) nanoparticles prepared under distinct synthesis conditions was assessed to oxidize imidacloprid (IMD) insecticide. After optimization of some operational variables, such as CuMF load (62.5-250 mg L-1), PMS concentration (250-1000 µM), and solution pH (3-10), IMD was completely oxidized in 2 h without interferences from leached metal ions. Such performance was also achieved when using tap water but was inhibited by a simulated municipal wastewater due to scavenging effects promoted by inorganic and organic species. Although there was evidence of the presence of sulfate radicals and singlet oxygen oxidizing species, only four intermediate compounds were detected by liquid chromatography coupled to mass spectrometry analysis, mainly due to hydroxyl addition reactions. Concerning the changes in surface properties of CuMF after use, no morphological or structural changes were observed except a small increase in the charge transfer resistance. Based on the changes of terminal surface groups, PMS activation occurred on Fe sites.

CoFe2O4 as a source of Co(II) ions for imidacloprid insecticide oxidation using peroxymonosulfate: Influence of process parameters and surface changes.

Nanometric cobalt magnetic ferrite (CoFe2O4) synthesized by distinct methods was used for in situ chemical activation of peroxymonosulfate (PMS) under neutral conditions to oxidize imidacloprid (IMD) insecticide. The effect of CoFe2O4 load (0.125-1.0 g L-1) and PMS concentration (250-1000 µM) was investigated as well as the influence of phosphate buffer and Co(II) ions. PMS activation by Co(II) ions, including those leached from CoFe2O4 (>50 µg L-1), exhibited a strong influence on IMD oxidation and, apparently, without substantial contributions from the solid phase. Within the prepared solid materials (i.e., using sol-gel and co-precipitation methods), high oxidation rates (ca. 0.5 min-1) of IMD were attained in ultrapure water. Phosphate buffer had no significant influence on the IMD oxidation rate and level, however, its use and solution pH have shown to be important parameters, since higher PMS consumption was observed in the presence of buffered solutions at pH 7. IMD byproducts resulting from hydroxylation reactions and rupture of the imidazolidine ring were detected by mass spectrometry. At optimum conditions (0.125 g L-1 of CoFe2O4 and 500 µM of PMS), the CoFe2O4 nanoparticles exhibited an increase in the charge transfer resistance and an enhancement in the surface hydroxylation after PMS activation, which led to radical (HO● and SO4●-) and nonradical (1O2) species. The latter specie led to high levels of IMD oxidation, even in a complex water matrix, such as simulated municipal wastewater at the expense of one-order decrease in the IMD oxidation rate.

Chemical composition and antifungal activity of the essential oil from the Hymenaea stigonocarpa Mart. Ex Hayne (jatobá-do-cerrado) fruit peel.

This study investigated the chemical composition and the antifungal activity of the essential oil extracted from the Hymenaea stigonocarpa fruit peel (HSFPEO) against Botrytis cinerea, Sclerotinia sclerotiorum, Aspergillus flavus and Colletotrichum truncatum. The HSFPEO obtained through hydrodistillation was analyzed with gas chromatography coupled to mass spectrometry. The antifungal activity was determined by the mean mycelial growth inhibition of the fungus treated with essential oils and growth control. The major constituents of HSFPEO were spathulenol (25.19%) and caryophyllene oxide (13.33%). HSFPEO demonstrated antifungal activity against all fungi tested in all concentrations evaluated in a dose-dependent behavior. The best results were observed against B. cinerea and A. flavus, in which the lowest concentration tested inhibited more than 70% of mycelial growth. Based on the current knowledge, this study describes for the first time the chemical composition and the antifungal activity of HSFPEO against the phytopathogenic fungi B. cinerea and C. truncatum.

Preparation and Characterization of a Coordination Polymer Based on Iron (III)-Cyamelurate as a Superior Catalyst for Heterogeneous Fenton-Like Processes.

We report on a new iron (iii)-cyamelurate-based coordination polymer. The new material based on a heptazine derivative was prepared in aqueous medium and characterized by a variety of techniques including TGA, FTIR, XRD, HRTEM, and STEM. Due to the high structural stability of the complex in aqueous media, its heterogeneous Fenton-like catalytic activity was evaluated using a model molecule. The results obtained showed a high catalytic activity in both in basic and acid media. The pseudo-first-order rate constants normalized by iron(III) concentrations was approximately 1000 times higher than the result obtained for traditional heterogeneous catalysts based on iron(III) oxyhydroxides. The best observed catalytic activities were attributed to the increase in the binding sites of Fe3+ ions, in parallel with the increased exposure of the catalytic sites, leading to a higher atomic efficiency of the reaction.

Exploring chemical diversity in Glycine max cultivars: A multivariate approach in the search for bioactive compounds against Spodoptera cosmioides.

Soybean crop is regulated by abiotic and biotic stresses with great potential in reducing grain yield and quality. The selection of resistant cultivars is a promising approach for mitigating these damages. We evaluated the chemical profile of Glycine max leaves from different cultivars in order to explore their defense mechanisms against Spodoptera cosmioides caterpillars. We optimized solid-liquid extraction techniques using ultrasound bath and static headspace extraction. Additionally, we developed an approach based on liquid and gas chromatography for analyzing the chemical profile of G. max cultivars. The principal component analysis allowed the classification of transgenic cultivars, which are classified as susceptible to S. cosmioides, from those obtained by genetic improvement and resistant to the insect. Differences were observed in the abundance of phenolic glycosides, lipids, aldehydes, and alcohols. More specifically, S. cosmioides resistant cultivars presented molecules related to the jasmonic and salicylic acid pathways. Such data can contribute to a molecular understanding of phenotypic diversity in soybean cultivars, from plant quality to resistance mechanisms and adaptation, to environmental stress and herbivory.

In vivo schistosomicidal activity of (±)-licarin A-loaded poly(ε-caprolactone) nanoparticles.

Schistosomiasis mansoni is an infectious parasitic disease caused by worms of the genus Schistosoma, and praziquantel (PZQ) is the medication available for the treatment of schistosomiasis. However, the existence of resistant strains reinforces the need to develop new schistosomicidal drugs safely and effectively. Thus, the (±)-licarin A neolignan incorporated into poly-Ɛ-caprolactone (PCL) nanoparticles and not incorporated were evaluated for their in vivo schistosomicidal activity. The (±)-licarin A -loaded poly(ε-caprolactone) nanoparticles and the pure (±)-licarin A showed a reduction in the number of worm eggs present in spleens of mice infected with Schistosoma mansoni. In addition, the (±)-licarin A incorporated in the concentration of 20 mg/kg and 200 mg/kg reduced the number of worms, presenting percentages of 56.3% and 41.7%, respectively.

Nanoparticles Loaded with Essential Oil from Zanthoxylum riedelianum Engl. Leaves: Characterization and Effects on Bemisia tabaci Middle-East Asia Minor 1.

Bemisia tabaci (Gennadius) (Hemiptera: Aleyrodidae) Middle-East Asia Minor 1 is a major pest of agricultural production systems. It is controlled by synthetic insecticides. Essential oils are promising eco-friendly alternatives. This study developed and characterized nanoparticles loaded with essential oils of Zanthoxylum riedelianum Engl. (Rutaceae) leaves and evaluated their potential for B. tabaci management. The essential oil exhibited an average yield of 0.02% (w w-1) and showed as major components γ-elemene (24.81%), phytol (18.16%), bicyclogermacrene (16.18%), cis-nerolidol (8.26%), and D-germacrene (6.52%). Characterization of the nanoparticles showed a pH between 4.5 and 6.7, a zeta potential of approximately - 25 mV, particle-size distribution ranging from 450 to 550 nm, and encapsulation efficiency close to 98%. The nanoencapsulation was an efficient process that provided photostability against photodegradation. Bioassays with crude and nanoencapsulated essential oils significantly reduced the number of nymphs and eggs of B. tabaci, with the best results observed at concentrations of 5 and 2% (v v-1). Our results demonstrated that essential oils from Z. riedelianum can be nanoformulated resulting in a stable product while maintaining their biological activity against B. tabaci Middle-East Asia Minor 1.

Characterization of Zanthoxylum rhoifolium (Sapindales: Rutaceae) Essential Oil Nanospheres and Insecticidal Effects to Bemisia tabaci (Sternorrhyncha: Aleyrodidae).

Encapsulation via nanotechnology offers a potential method to overcome limited thermal and photo-stability of botanical pesticides. In this study, nanospheres of essential oils (NSEO) derived from Zanthoxylum rhoifolium Lam. fruit were characterized and evaluated for their photostability and insecticidal activity against Bemisia tabaci. Three major compounds of Z. rhoifolium fruits were detected by CG-MS: ß-phellandrene (76.8%), ß-myrcene (9.6%), and germacrene D (8.3%). The nanoprecipitation method was used to obtain homogeneous spherical NSEO, with ≥98% encapsulation efficiency. Tests with UV/Vis spectrophotometry showed significantly reduced photodegradation from exposed NSEO samples when compared with essential oil (EO) controls. Whitefly screenhouses bioassays with bean plants treated with 0.25, 0.5, 1 and 1.5% suspensions showed EO treatments in both free and nanoencapsulated forms reduced adult whitefly oviposition by up to 71%. In further tests, applications at 1.5% caused ≥64% mortality of second instar nymphs. When the test was conducted under high temperature and light radiation conditions, the insecticidal effect of NSEO treatments was improved (i.e., 84.3% mortality) when compared to the free form (64.8%). Our results indicate the insecticidal potential of EO-derived from Z. rhoifolium fruits with further formulation as nanospheres providing greater photostability and enhanced insecticidal activity against B. tabaci under adverse environmental conditions.

Morphological and chemical plant traits associated with feeding non-preference to adult of Diabrotica speciosa (Coleoptera: Chrysomelidae) in soybean genotypes.

Diabrotica speciosa is an important pest of several crops in South America, including soybeans. Adults cause severe defoliation in soybean plants, and damage is significant when cotyledons are attacked. This study evaluated feeding non-preference to D. speciosa adults using 10 soybean genotypes, testing (i) 15-day-old whole plants and (ii) leaf disks of 60-day-old plants, through assessments of soybean attractiveness and leaf area consumed (LAC). Foliar contents of flavonoids and nutrients, and leaf trichome density were quantified for potential correlations with soybean resistance to adult of D. speciosa. In the whole young-plant experiment, under free-choice conditions, the lowest LAC was observed in IAC 100 and PI 227687. In no-choice, PI 227687 and IGRA RA 626 RR showed lower LAC than the other genotypes. In the leaf disk test, in free-choice, the genotypes IAC 100, PI 274454, PI 227687, DM 339, and BR 16 were the least preferred by adult of D. speciosa. In no-choice, PI 274454 was one of the least preferred, similarly to IGRA RA 626 RR, Dowling, and PI 227687. In the whole plant experiment, a high rutin content and low amounts of zinc, calcium, sulfur and manganese were associated with less consumption of D. speciosa on leaves of resistant genotypes. In contrast, in the leaf disk test there was a significant influence of trichomes in soybean resistance to the pest. In conclusion, the PI lines herein assessed are also promising sources for developing cultivars resistant to D. speciosa.

The Symbiotic Fungus Leucoagaricus gongylophorus (Möller) Singer (Agaricales, Agaricaceae) as a Target Organism to Control Leaf-Cutting Ants.

Atta and Acromyrmex are the main genera of leaf-cutting ants present in North and South America, causing extensive damage to agroforestry. Control of the ants requires high handling costs with few effective methods available to decrease the losses. The symbiosis between the leaf-cutting ants and the fungus Leucoagaricus gongylophorus is essential for ant nest survival. Therefore, L. gongylophorus may be a key target in controlling leaf-cutting ants, since its reduction may cause an imbalance in the symbiosis necessary to maintain the nest. Among the options for natural fungal control, plant species are considered important sources of compounds belonging to several classes of natural products that show potential as antifungal agents. This review also presents studies that establish that the antagonist fungi from the Escovopsis and Trichoderma genera effectively reduce the development of L. gongylophorus. The development of nanostructured delivery systems, which have shown advantages over conventional formulations, is suggested for ant control; no commercial nanotechnology-based product has yet been developed, and this appears to be a new approach for future studies.

Evaluation of lignan-loaded poly(ε-caprolactone) nanoparticles: synthesis, characterization, in vivo and in silico schistosomicidal activity.

Lignan dinitrohinokinin displays important biological activities, which led to the preparation of its poly-ε-caprolactone nanoparticles. Kinetics analysis revealed initially slow drug release followed by a prolonged, moderate release 6 h later due to DNHK diffusion through the polymeric matrix. Molecular dynamics simulations show that DNHK molecules that interact stronger with other DNHK molecules near the PCL/DNHK surface are more difficult to dissociate from the nanoparticle. The smaller diameter nanocapsules with negative surface charge conferred good colloidal stability. The formulations showed a size distribution with monodisperse systems formation. In vivo evaluation of schistosomicidal activity against Schistosoma mansoni showed that DNHK, when incorporated into nanoparticles, caused egg number reduction of 4.2% and 28.1% at 40 mg/kg and 94.2% and 84.4% at 400 mg/kg in the liver and the spleen, respectively. The PCL nanoparticles were stable in aqueous dispersion and could be optimized to be used as a promising lignan release agent.

Insecticidal activity of copper (II) complexes with flavanone derivatives.

In this work, we describe the insecticidal activity against Spodoptera frugiperda of flavanone derivatives (naringin, naringenin and hesperidin) complexed to copper (II). For the assays, the compounds were incorporated into an artificial diet and offered to S. frugiperda during its larval period. The duration of larval and pupal phases, the weight of pupae and the percentage of dead insects at the end of the larval phase were evaluated. Among the tested compounds, the free flavanones 1 and 3 and the complexes 4 and 6 showed a shortening of the larval phase when compared to the control. Complex 9 showed the highest toxicity, with 96.66% larval mortality. This is the first report on the insecticidal activity of the Cu2+ complexes of the flavanones naringin, naringenin and hesperidin.[Formula: see text].

Chemical composition and antifungal activity of Zanthoxylum riedelianum stem bark essential oil.

The phytopathogenic fungi Sclerotinia sclerotiorum and Rhizopus stolonifer infect different crop plants. Essential oils have been used as an alternative to chemical control methods. Therefore, the objective of this study was to analyze the essential oil chemical composition of the stem bark of Zanthoxylum riedelianum (ZREO) and evaluate its antifungal potential. The ZREO obtained by hydrodistillation was analyzed using gas chromatography coupled to mass spectrometry and evaluated for in vitro antifungal activity. The major components identified in the chemical analysis were E-nerolidol (67.21%), α-selinene (14.94%), and ß-selinene (7.41%). The antifungal potential of ZREO against S. sclerotiorum and R. stolonifer was detected at all concentrations evaluated in a dose-dependent manner. The best results were against R. stolonifer, with the concentration of 150 µLmL-1 inhibiting more than 80% of mycelial growth. On the basis of the current knowledge, this study describes for the first time the chemical composition and their antifungal activity.

Solvent Mixture Optimization in the Extraction of Bioactive Compounds and Antioxidant Activities from Garlic (Allium sativum L.).

Garlic is a health promoter that has important bioactive compounds. The bioactive extraction is an important step in the analysis of constituents present in plant preparations. The purpose of this study is to optimize the extraction with the best proportion of solvents to obtain total phenolic compounds (TPC) and thiosulfinates (TS) from dried garlic powder, and evaluate the antioxidant activities of the optimized extracts. A statistical mixture simplex axial design was used to evaluate the effect of solvents (water, ethanol, and acetone), as well as mixtures of these solvents, after two ultrasound extraction cycles of 15 min. Results showed that solvent mixtures with a high portion of water and pure water were efficient for TPC and TS recovery through this extraction procedure. According to the regression model computed, the most significant solvent mixtures to obtain high TPC and TS recovery from dried garlic powder are, respectively, the binary mixture with 75% water and 25% acetone and pure water. These optimized extracts presented oxygen radical absorbance capacity. Pure water was better for total antioxidant capacity, and the binary mixture of water-acetone (75:25) was better for DPPH scavenging activity. These optimized extracts can be used for industrial and research applications.

Encapsulation of B. bassiana in Biopolymers: Improving Microbiology of Insect Pest Control.

The fungus Beauveria bassiana is widely used for pest control; however, biostability and dispersion for broth pulverization are limiting factors for its application in the field. In this context, formulation techniques such as microencapsulation are viable alternatives. The aim of this work is to optimize B. bassiana formulations by spray dryer and evaluate its stability and biological activity against Spodoptera cosmioides compared to ionic gelatinization formulations. The fungus was biocompatible with all evaluated biopolymers (lignin, cellulose, starch, humic substances, and alginate). The encapsulation by spray drying was optimized by factorial design in an inlet and outlet air temperature of 120°C and 68°C, respectively; aspirator rate of 35 m3·h-1, feed flow rate of 12 mL·min-1; and drying gas flow at 35 L·h-1. The ionic gelation capsules were obtained using a 0.5% quantity of conidia in a 1% sodium alginate solution dropped into a 0.5 mol·L-1 CaCl2 solution using a peristaltic pump. Spray drying provided smaller microcapsules than those by ionic gelation. Both techniques produced more stable conidia when exposed to temperature and UV-radiation than non-formulated B. bassiana. The formulations prepared by spray drying showed gains at aqueous dispersion. Biological assays against Spodoptera cosmioides showed a mortality rate of up to 90%. These results demonstrate the suitability of encapsulating B. bassiana conidia stably in aqueous dispersion without loss of viability and virulence.

Design of experiments applied to stress testing of pharmaceutical products: A case study of Albendazole.

Forced degradation tests are studies used to assess the stability of active pharmaceutical ingredients (APIs) and their formulations. These tests are performed submitting the API under extreme conditions in order to know the main degradation products in a short period of time. The results of these studies are used to assess the degradation susceptibility of APIs and to validate chromatographic analytical methods. However, most of degradation studies are performed using one-factor-at-the-time (OFAT) which does not consider the interactions between degradation variables. This work proposes the use of Design of Experiment (DoE) approach in forced degradation of albendazole (ABZ). It was used a central composite design (CCD) to evaluate the forced degradation in a multivariate way. Experiments were performed taking into account the variables pH, temperature, oxidizing agent (H2O2) and UV radiation. It was verified the influence of the variables and their interactions on the ABZ degradation. The ABZ oxidation showed to be the main degradation route for ABZ, which is strongly influenced by the temperature. The hydrolysis was relevant at alkaline medium and high temperature. LC-IT-MSn was used to identify the degradation products. It was found three known degradation products (albendazole-2-amino, albendazole sulfoxide and albendazole sulfone) and a new derivate of albendazole molecule (albendazole sulfoxide with a chlorine). This last one was isolated and characterized by UPLC-QToF-MS and NMR analyses.

Endophytic bacteria from strawberry plants control gray mold in fruits via production of antifungal compounds against Botrytis cinerea L.

Botrytis cinerea causes the gray mold disease in a wide range of plant hosts, especially in post-harvest periods. The control of this phytopathogen has been accomplished through the application of fungicides. However, this practice can cause environmental problems and increase fruit production costs. In addition, this fungus species has developed resistance to conventional synthetic fungicides. In this context, plant growth-promoting bacteria have shown potential for application in agricultural production because they are able to stimulate plant growth through different mechanisms, including the biological control of phytopathogens (indirect growth promotion mechanism). The aim of this work was to evaluate in vitro and in fruits the potential for indirect plant growth-promotion of bacteria isolated from strawberry leaves and roots. Dual plate method and inverted plate method were used to verify the ability of controlling in vitro the growth of Botrytis cinerea via the production of diffusible and volatile antifungal compounds, respectively. The effect of six bacterial isolates that showed greater potential for biological control in vitro was evaluated by scanning electron microscopy. Antifungal compounds produced by these bacterial isolates were identified by liquid chromatography coupled with mass spectrometry. Six bacterial strains were tested on strawberry pseudofruits. Five selected strains belong to the genus Bacillus and one to the genus Pantoea sp. Selected strains were able to inhibit more than 80 % of the mycelial growth of B. cinerea by the production of diffusible compounds and 90 % by volatile antifungal compounds production. Scanning electron microscopy showed the intense degradation of fungal hyphae caused by the presence of all bacterial strains. Bioactive compounds (salycilamide, maculosin, herniarin, lauroyl diethanolamide, baptifoline, undecanedioic acid, botrydial, 8 3-butylidene-7-hydroxyphthalide and N-(3-oxo-henoyl)-homoserine lactone) were obtained from liquid culture of these strains and extraction with ethyl acetate. All six isolates tested in vivo reduced the incidence of gray mold in strawberry pseudofruits in postharvest. It is concluded that isolates 26, 29, 65, 69, 132 (Bacillus sp.) and MQT16M1 (Pantoea sp.) have potential application for the biological control of Botrytis cinerea in strawberry via the production of diffusible and volatile antifungal compounds.

Octahedral ruthenium and magnesium naringenin 5-alkoxide complexes: NMR analysis of diastereoisomers and in-vivo antibacterial activity against Xylella fastidiosa.

Although many copper-based antimicrobial compounds have been developed to control pathogenic bacteria and fungi in plants and applied for crop protection, there is evidence that several plant pathogens have developed resistance to copper-based antimicrobial compounds, including some Xanthomonas species. Xylella is a bacterial genus belonging to the Xanthomonas family; and X. fastidiosa, which is responsible for citrus variegated chlorosis (CVC) in sweet orange, may develop resistance to one or more copper-based antimicrobials. Because of the time required for the development and approval of new antimicrobials for commercial use, the discovery of novel bactericidal compounds is essential before the development of resistance to the antimicrobials currently in use becomes widespread. Here, we explored the antimicrobial potential of two newly synthesized antimicrobials complexes and one natural compound against X. fastidiosa. Several nuclear magnetic resonance (NMR) assays with high resolution and sensitivity were developed to identify new diastereoisomers in the context of octahedral ruthenium - [Ru(narin)(phen)2]PF6-and magnesium naringenin 5-alkoxide - [Mg(narin)(phen)2]OAc - complexes, obtained in the present work. The NMR assays proved to be powerful tools for the identification of isomers in metal complexes. Moreover, a protocol for the in-vivo determination of the effects of these complexes against X. fastidiosa was developed. The main trunks of X. fastidiosa infected plants were injected with the two complexes as well as with the limonoid azadirachtin using a syringe; the number of bacterial cells in the plants following treatment was estimated via real-time quantitative PCR (qPCR). Importantly, the administration of both complexes and of azadirachtin drastically reduced the number of X. fastidiosa cells in vivo.

Avocado kernels, an industrial residue: a source of compounds with insecticidal activity against silverleaf whitefly.

Fruit processing waste, such as kernels (endocarp + seed) of avocado [Persea americana Mill. (Lauraceae)], could be used as raw material in the preparation of botanical insecticides. In light of this potential, this study assessed the insecticidal action of extracts and fractions from kernels of two avocado cultivars (Breda and Margarida) on Bemisia tabaci (Gennadius) (Hemiptera: Aleyrodidae) biotype B, an important pest species in tropical conditions. Ethanolic and aqueous extracts prepared from kernels of P. americana, regardless of the plant cultivar used, caused promising insecticidal activity to whitefly nymphs. Based on yield in crude extracts [10.32 and 9.85% (w/w), respectively, for cultivars Breda and Margarida], on the bioassay results with crude extracts and on the chemical profiles, the ethanolic extract of kernels of P. americana cv. Breda was chose for the continuation of the study. Thus, the ethanolic extract of kernels of cv. Breda (LC50 = 197.84 ppm and LC90 = 567.19 ppm) was selected and subjected to fractionation by the liquid-liquid partition technique. The hexane and dichloromethane fractions of this extract caused significant mortality of nymphs. The analysis using the ultraviolet (UV) and hydrogen nuclear magnetic resonance (1H NMR) showed the presence of long-chain aliphatic compounds (alkanols or acetogenins of Lauraceae), alkylfurans (or avocadofurans), and unsaturated fatty acids in these fractions, which are possibly related to bioactivity observed in B. tabaci, besides saccharides. The results show that kernels of P. americana are promising sources of compounds with insecticidal action for the control of B. tabaci biotype B, a great opportunity to transform environmental problems into eco-friendly solutions to agriculture.

Evaluation of the microencapsulation of orange essential oil in biopolymers by using a spray-drying process.

Essential oils are volatile compounds commonly used by several industries, easily degradable, which restrains their applications. Therefore, we developed and validated a methodology for producing microcapsules loaded with orange essential oil, using a spray-drying process. The experimental design results showed that the combination between a low flow transfer rate (0.15 L h-1) of the colloidal suspension, a higher drying air flow rate (536 L h-1), and an inlet air temperature of 150 °C to the spray-dryer were the most important parameters for the atomization efficiency. The method optimization resulted in microcapsules with powder recovery between 7.6 and 79.9% (w w-1), oil content ranging from 8.9 to 90.4% (w w-1), encapsulation efficiency between 5.7 and 97.0% (w w-1), and particle sizes with a high frequency of distribution less than 4 µm. In these experiments, gelatin and lignin were evaluated as biopolymers of encapsulation. We also developed an analytical method using headspace gas chromatography. The matrix effects could be addressed by using matrix-matched calibration curves. The chromatographic analysis was linear and selective for D-limonene between 0.025 and 3.00 µg mL-1, with correlation coefficients higher than 0.99. The analytical method had limits of detection and quantitation of 0.024 and 0.073 mg g-1 for gelatin and 0.039 and 0.119 mg g-1 for lignin, respectively.