Simultaneous analysis of pesticides and mycotoxins in primary processed foods: The case of bee pollen.

Primary Processed Foods are a class of food items that are ready for consumption after minimal processing in the supply chain. These products are ubiquitous in our daily diet, but so far a limited number of studies dealt with the optimization of quality control methods to check their content of contaminants. Among primary processed foods, bee pollen is a nutritionally acclaimed food supplement, whose contamination with pesticides and mycotoxins has been largely proven. For this reason, the present study aimed at optimizing for the first time a comprehensive LC-MS/MS method capable of analyzing 282 pesticides and 8 mycotoxins in bee pollen. To obtain a suitable method, two extraction procedures (QuEChERS and Accelerated Solvent Extraction), as well as different chromatographic gradients and columns, were tested. The optimized methodology, comprehending an extraction based on semi-automated QuEChERS, and an analytical method including inert LC column technology, was validated and applied to a sample set of 34 bee pollens. The analyzed samples collectively showed the presence of 41 pesticides and 1 mycotoxin.

[Pulmonary Embolism]. / Tromboembolia de pulmón.

Pulmonary embolism (PE), the most severe form of presentation of venous thromboembolic disease (VTE), currently represents a foremost healthcare issue due to its high impact in terms of morbidity, mortality, costs, and resource consumption. Early mortality associated with PE is primarily due to hemodynamic instability, exacerbation of pre-existing conditions, or major complications of antithrombotic therapies. Beyond the risk of death, there are relevant complications related to PE, such as bleedings, VTE recurrences, and persistence of residual respiratory symptoms; the latter complication related to PE is mainly characterized by two entities, chronic thromboembolic pulmonary hypertension and chronic thromboembolic disease. Significant scientific advances made in recent years have allowed for the improvement of both diagnostic and therapeutic management of the disease, as outlined in this document through a series of relevant issues about PE that are answered with the most up-to-date scientific evidence.

Peri-implantitis and maxillary sinus membrane thickening: A retrospective cohort study.

OBJECTIVE: The objective of this study is to investigate the association of peri-implantitis (PI) and sinus membrane thickening and to assess the resolution of membrane thickening following intervention (implant removal or peri-implantitis treatment) aimed at arresting PI. MATERIALS AND METHODS: Forty-five patients with 61 implants in the posterior maxillary region were retrospectively included in the study. Twenty-four patients were diagnosed with peri-implantitis (PI) and 21 had peri-implant health (PH). Cone-beam computed tomography (CBCT) scans were evaluated to assess maxillary sinus characteristics, including membrane thickening, sinus occupancy and ostium patency. The CBCT scans taken 6 months after intervention aimed at arresting disease (implant removal or treatment of PI) in the PI group were also appraised and compared to baseline scans. RESULTS: At baseline, all parameters evaluating membrane thickness disorders yielded significant differences between groups (p < .001). Patients with posterior maxillary implants diagnosed with PI were 7× more likely to present membrane thickening compatible with pathology when compared to patients with healthy implants (OR = 7.14; p = .005). Furthermore, the likelihood was 6x greater in implants diagnosed with PI to exhibit moderate membrane thickening (OR = 6.75, p = .001). The patients receiving interventions aimed at arresting PI experienced significant enhancement in all radiographic parameters related to the sinus cavity at the 6-month follow-up (p < .001), though these variations were similarly independent of whether treatment consisted of PI treatment or implant removal. CONCLUSIONS: Maxillary sinus membrane thickening and the permeability/obstruction of the ostium are frequently associated with the presence of PI in posterior implants. Interventions targeting disease resolution effectively reduce membrane thickness to levels compatible with maxillary sinus health.

The role of food during oncology treatment: perspectives of cancer patients, caregivers and healthcare professionals.

PURPOSE: Many cancer patients have problems eating which are usually connected to taste and smell alterations due to side effects of cancer treatment. These problems have consequences both in terms of malnutrition and reduced quality of life. In order to explore social and psychological consequences of eating problems in cancer patients, qualitative interviews were conducted with cancer patients, their caregivers and healthcare professionals. METHODS: The study was conducted in three European countries (Poland, Spain and the UK) that differed in culture, oncology care approaches and availability of nutritional products targeted to cancer patients in the market. RESULTS: Differences in the social role of eating between the three European countries were observed which subsequently influenced the impact of eating problems for cancer patients in these countries. Furthermore, the study found that problems with food affect not only the quality of life of cancer patients, but can also distress their caregivers, who are often unable to cope with such food-related problems. In addition, the study showed that commercially available nutritional products for cancer patients focus on nutritional value but tend to neglect an important aspect of eating, which is the enjoyment of food, both individually and socially.

Sphingomyelinase-responsive nanomicelles for targeting atherosclerosis.

Atherosclerosis, a leading cause of cardiovascular diseases requires approaches to enhance disease monitoring and treatment. Nanoparticles offer promising potential in this area by being customisable to target components or molecular processes within plaques, while carrying diagnostic and therapeutic agents. However, the number of biomarkers available to target this disease is limited. This study investigated the use of sphingomyelin-based nanomicelles triggered by sphingomyelinase (SMase) in atherosclerotic plaques. Accumulation of iron oxide-based nanomicelles in the plaque was demonstrated by fluorescence, MR imaging and electron microscopy. These findings demonstrate the possibility of utilising SMase as a mechanism to retain nanoprobes within plaques, thus opening up possibilities for future therapeutic interventions.

Vascular Delay Soft Tissue Technique in Oral/Maxillary Bone Reconstructive Surgery: A Technical Note.

PURPOSE: The present study describes a new presurgical soft tissue technique in oral/maxillary bone reconstructive surgery for reducing the risk of soft tissue dehiscence and its related complications. MATERIALS AND METHODS: Ten consecutive patients with Cawood and Howell type V atrophy were scheduled for CAD/CAM titanium mesh bone reconstructive surgery after applying the vascular delay technique 21 days before regenerative surgery. The surgical and healing complications were clinically assessed at nine time points, ranging from the time of bone regenerative surgery to 9 months after surgery. Surgical complications included flap damage and neurologic and vascular complications. Healing complications were subdivided into four classes. These classes comprised Class I: small membrane exposure (≤ 3 mm) without purulent exudate; Class II: large membrane exposure (> 3 mm) without purulent exudate; Class III: membrane exposure with purulent exudate; and Class IV: abscess formation without membrane. RESULTS: The study sample included seven men and three women (mean age: 48.2 ± 3.5 years) with seven mandibular cases and three maxillary cases. The defect length ranged from three to six teeth, with a mean mesiodistal distance of 29.9 ± 8.5 mm and a mean volume augmentation of 2.03 ± 0.9 cm3. There were no surgical complications. One patient presented a Class I healing complication that did not affect the regeneration outcome. CONCLUSIONS: The vascular delay technique appears to reduce the risk of soft tissue dehiscence and exposure in bone regenerative surgery, though randomized studies involving larger samples and longer follow-up periods are needed in order to draw firm conclusions.

Effectiveness of virtual reality in relieving anxiety and controlling hemodynamics during oral surgery under local anesthesia: A prospective randomized comparative study.

It was the aim of the study to evaluate the contribution of a relaxing immersive experience with virtual reality (VR) goggles in reducing patient anxiety related to wisdom tooth extraction under local anesthesia. A prospective randomized comparative study in consecutive patients scheduled for bilateral wisdom tooth extraction under local anesthesia was carried out between March and December 2022. Both sides were operated upon in the same surgery, but on one side VR goggles were applied (VR), while on the other they were not (noVR). Anxiety was evaluated both subjectively (State-Trait Anxiety Inventory [STAI] and visual analogue scale [VAS]) and objectively (measuring heart rate, blood pressure [BP] and blood oxygen saturation) before (T1) and after each surgical step (T2VR and T2noVR). The study sample consisted of 27 patients: 9 men and 18 women, with an average age of 25.8 ± 6.5 years (range: 18-43). Anxiety as assessed by the STAI and VAS decreased from T1 to T2 (p < 0.001 and p < 0.001, respectively), although to a similar degree regardless of whether VR was used or not. Heart rate showed significant differences influenced by RV exposure (p = 0.013): it increased +2.5 ± 8.8 bpm in the control group and decreased -2.22 ± 7.55 bpm with VR (p = 0.013). Both minimum and maximum BP after surgery were significantly higher in the noVR group (p = 0.002 and p = 0.040, respectively). Regarding minimum BP, VR proved more effective among male patients (p = 0.057) and on starting the procedure using VR (p = 0.055). The results provided evidence of meaningful control of the hemodynamic variables, but less predictable performance in the subjective evaluation of anxiety.

Evaluation of the sorption/desorption processes of pesticides in biodegradable mulch films used in agriculture.

Microplastics from mulch films can be a source of chemical contamination to agricultural soils. In this context, biodegradable films have been widely positioned as a greener choice. However, their sorption/desorption capabilities, in contrast to the conventional plastic types remain understudied. It is for this reason that objective evaluation of their interactions with residual agricultural contaminants becomes important. Our findings reveal that polyethylene (PE) mulch films retained lower amounts of pesticide residues and demonstrated a higher desorption/release [median desorption = 71.86 µg/L or about 50%], while polybutylene adipate terephthalate (PBAT) mulch films retained higher amounts of pesticide residues onto their surface and demonstrated a much lower desorption [median desorption = 24.27 µg/L or about 17%] after a spraying event. A higher ambient temperature had no significant effect on final desorption amounts in both PE [median = 65.27 µg/L at 20 °C and 74.23 µg/L at 40 °C] and PBAT [median = 24.26 µg/L at 20 °C and 24.78 µg/L at 40 °C] mulch films. However, it did favour a faster desorption pace in PE films. Desorption in PBAT and PE plastic types was correlated with the log Kow value [Spearman's correlation: 0.857 and 0.837 respectively, p < 0.05]. However, only a moderate correlation with pKa was observed in PBAT [Spearman's correlation: 0.478, p < 0.05], while none for PE plastic type. Sorption of pesticides onto biodegradable PBAT microplastics were best explained by Elovich [R2: 0.937-0.959] and pseudo-second order kinetics [R2: 0.942-0.987], suggesting the presence of chemisorption. Furthermore, Weber Morris plots suggested the presence of a multi-step process and Boyd plots indicated that film diffusion or chemical bond formation was the rate-limiting step governing this phenomenon.

Disease severity-based subgrouping of type 2 diabetes does not parallel differences in quality of life: the Maastricht Study.

AIMS/HYPOTHESIS: Type 2 diabetes is a highly heterogeneous disease for which new subgroups ('clusters') have been proposed based on disease severity: moderate age-related diabetes (MARD), moderate obesity-related diabetes (MOD), severe insulin-deficient diabetes (SIDD) and severe insulin-resistant diabetes (SIRD). It is unknown how disease severity is reflected in terms of quality of life in these clusters. Therefore, we aimed to investigate the cluster characteristics and cluster-wise evolution of quality of life in the previously defined clusters of type 2 diabetes. METHODS: We included individuals with type 2 diabetes from the Maastricht Study, who were allocated to clusters based on a nearest centroid approach. We used logistic regression to evaluate the cluster-wise association with diabetes-related complications. We plotted the evolution of HbA1c levels over time and used Kaplan-Meier curves and Cox regression to evaluate the cluster-wise time to reach adequate glycaemic control. Quality of life based on the Short Form 36 (SF-36) was also plotted over time and adjusted for age and sex using generalised estimating equations. The follow-up time was 7 years. Analyses were performed separately for people with newly diagnosed and already diagnosed type 2 diabetes. RESULTS: We included 127 newly diagnosed and 585 already diagnosed individuals. Already diagnosed people in the SIDD cluster were less likely to reach glycaemic control than people in the other clusters, with an HR compared with MARD of 0.31 (95% CI 0.22, 0.43). There were few differences in the mental component score of the SF-36 in both newly and already diagnosed individuals. In both groups, the MARD cluster had a higher physical component score of the SF-36 than the other clusters, and the MOD cluster scored similarly to the SIDD and SIRD clusters. CONCLUSIONS/INTERPRETATION: Disease severity suggested by the clusters of type 2 diabetes is not entirely reflected in quality of life. In particular, the MOD cluster does not appear to be moderate in terms of quality of life. Use of the suggested cluster names in practice should be carefully considered, as the non-neutral nomenclature may affect disease perception in individuals with type 2 diabetes and their healthcare providers.

Symptom-related screening programme for early detection of chronic thromboembolic pulmonary hypertension after acute pulmonary embolism: the SYSPPE study.

BACKGROUND: Chronic thromboembolic pulmonary hypertension (CTEPH) is the most severe long-term complication of acute pulmonary embolism (PE). We aimed to evaluate the impact of a symptom screening programme to detect CTEPH in PE survivors. METHODS: This was a multicentre cohort study of patients diagnosed with acute symptomatic PE between January 2017 and December 2018 in 16 centres in Spain. Patients were contacted by phone 2 years after the index PE diagnosis. Those with dyspnoea corresponding to a New York Heart Association (NYHA)/WHO scale≥II, visited the outpatient clinic for echocardiography and further diagnostic tests including right heart catheterisation (RHC). The primary outcome was the new diagnosis of CTEPH confirmed by RHC. RESULTS: Out of 1077 patients with acute PE, 646 were included in the symptom screening. At 2 years, 21.8% (n=141) reported dyspnoea NYHA/WHO scale≥II. Before symptom screening protocol, five patients were diagnosed with CTEPH following routine care. In patients with NYHA/WHO scale≥II, after symptom screening protocol, the echocardiographic probability of pulmonary hypertension (PH) was low, intermediate and high in 76.6% (n=95), 21.8% (n=27) and 1.6% (n=2), respectively. After performing additional diagnostic test in the latter 2 groups, 12 additional CTEPH cases were confirmed. CONCLUSIONS: The implementation of this simple strategy based on symptom evaluation by phone diagnosed more than doubled the number of CTEPH cases. Dedicated follow-up algorithms for PE survivors help diagnosing CTEPH earlier. TRIAL REGISTRATION NUMBER: NCT03953560.

Does Aesthetic Osseous Genioplasty Impact Upper Airway Volume?

BACKGROUND: Although maxillomandibular advancement is the treatment of choice for obstructive sleep apnea syndrome (OSAS) in the presence of underlying maxillomandibular complex hypoplasia, there is still a gap in the literature regarding the impact of genioplasty upon upper airway volume (UAV). OBJECTIVES: The aim of this study was to evaluate the impact of isolated osseous genioplasty upon UAV. METHODS: A retrospective analysis of all patients subjected to isolated osseous genioplasty between July 2015 and July 2022 was conducted. Cone-beam computed tomography was performed preoperatively and postoperatively to assess the chin and hyoid 3-dimensional (3D) spatial position and UAV changes after surgery. RESULTS: A total of 44 patients were included in the study. Regarding surgical movements of the chin, almost all patients received a sagittal movement (n = 42; 39 forward and 3 backward), while in 8 patients a vertical movement (5 upward and 3 downward) was applied, and in 6 patients the chin was centered. Statistically significant increases in total UAV (P = .014) and at the level of the oropharynx (P = .004) were observed. Specifically, chin centering, upward and forward movements enlarged the oropharynx volume (P = .006, .043 and .065, respectively). Chin advancement enlarged the hypopharynx volume (P = .032), as did upward movement of the hyoid bone (P < .001). CONCLUSIONS: Results of the study suggest that aesthetic osseous genioplasty impacts the UAV: each 3D spatial chin movement differently impacts the upper airway by enlarging or narrowing it. However, further studies addressing the apnea-hypopnea index are required to assess its effectiveness in treating OSAS.

Quantification of nanoplastic uptake and distribution in the root, stem and leaves of the edible herb Lepidum sativum.

This study confirms the uptake, translocation and bioaccumulation of 100 nm polystyrene nanoplastics in the root, stem and leaves of the plant Lepidum sativum at exposure concentrations ranging from environmentally realistic 10 µg/L up to a high of 100 mg/L. Accumulation in plant tissues was characterised by aggregation in the intercellular spaces and heterogeneous distribution. Nanoplastic presence was confirmed in the root tips, root surface and stele, lateral roots, root hairs, stem vascular bundles, leaf veins and mesophyll, as well as leaf epidermis including stomatal sites. Quantification results show that majority of the particles were retained in the root and accumulation in stem and leaves was only 13 to 18 % of the median value in roots. There was a reduction of 38.89 ± 9.62 % in the germination rate, 55 % in plant fresh weight, as well as in root weight (> 80 %), root length (> 60 %), shoot weight (51 to 78 %) and number of lateral roots (> 28 %) at exposure concentrations at and above 50 mg/L. However, lower, environmentally probable exposure concentrations did not affect the plant health significantly. Our results highlight the urgent need for further exploration of this issue from the point of view of food safety and security. STATEMENT OF ENVIRONMENTAL IMPLICATION: Micro and nanoplastics have been reported in agricultural environments across the globe and reports regarding their hazardous effects over agricultural and plant health call for an urgent exploration of this issue. This work demonstrates the uptake, bioaccumulation and distribution of nanoplastics in an edible plant at an environmentally realistic concentration and raises serious concerns regarding the possible implications for food safety and security. It presents a novel approach which addresses the quantification of nanoplastic accumulation in plant tissues and helps identify the mechanism and trends behind this phenomenon which has been a challenge up until now.

Method optimisation for large scope pesticide multiresidue analysis in bee pollen: A pilot monitoring study.

Pesticide contamination in emerging foods and supplements is currently a topic of great interest. This study focused on the evaluation of pesticide residues in commercial bee pollen samples to evaluate the risk associated with their consumption. To this end, an automated clean-up method for the pesticide extracts of bee pollen was developed. An LC-MS/MS and a GC-MS/MS method were validated for the analysis of 353 pesticides in 80 bee pollen samples purchased from different countries. The results showed the presence of 77 different pesticide residues in bee pollen, including plant protection chemicals and veterinary treatments. 85 % of the samples were contaminated with pesticides and no relevant differences were found between conventional and organic samples. Pesticide concentrations exceeding the imposed MRL were found in 40 % of the samples, but the risk assessment showed that consumers are not exposed to an unacceptable risk when consuming the evaluated bee pollen.

Pulmonary embolism: a practical approach to update risk stratification and treatment decisions based on the guidelines.

INTRODUCTION: Pulmonary embolism (PE) is a prevalent condition with a substantial morbi-mortality worldwide. Proper risk stratification of PE is essential for identifying the most suitable therapeutic strategy and the optimal care setting for the patient. This process entails evaluating various factors, including symptoms, comorbidities, and right heart dysfunction. AREAS COVERED: This review assesses the tools and methods utilized to identify and stratify individuals based on the probability of developing deterioration or death related to PE. Current guidelines divide PE into three groups: high-risk (previously termed massive) PE, intermediate-risk (sub-massive) PE, and low-risk PE. Various risk scores, such as the simplified pulmonary embolism severity index (sPESI), Bova score, and the FAST score (incorporating Heart-Fatty Acid binding protein [H-ABP], Syncope, Tachycardia), aid in identifying patients at higher risk. Additionally, the Hestia score is instrumental in pinpointing low-risk patients. EXPERT OPINION: Presently, there is a dearth of high-quality frameworks for the optimal management and treatment of PE patients at risk of hemodynamic collapse. A consortium of experts is in the process of formulating a new conceptual model for risk stratification, taking into account a comprehensive array of variables and outcomes to facilitate more individualized management of acute PE.

Final-year medical students' perspective: a survey on the use of computed tomography in sepsis.

OBJECTIVES: To determine the perspective of final-year medical students on the use of computed tomography (CT) in patients with sepsis. METHODS: A total of 207 questionnaires were distributed to final-year medical students at a large university medical center, and 113 returned questionnaires met the criteria for inclusion in the analysis. Questions referred to sepsis guidelines, CT indications, and the use of contrast agents. Control variables included a level of practical experience as a final-year student (trimester of student's practical year) and previous radiological experience. Statistical hypothesis tests such as the Mann-Whitney U test and chi-square test were performed. RESULTS: The majority of participating students, 85% (n = 91/107), considered a Systemic Organ Failure Assessment (SOFA) score ≥ 2 as a diagnostic criterion for sepsis. The presence of ≥ 2 positive systemic inflammatory response syndrome (SIRS) criteria was considered relevant for diagnosing sepsis by 34% (n = 34/100). Ninety-nine percent (n = 64/65) of the participants who fully agreed with a SOFA score ≥ 2 being relevant for diagnosing sepsis would also use it as an indication for a CT scan. Seventy-six percent (n = 78/103) of the students rated a known severe allergic reaction to contrast agents as an absolute contraindication for its administration. Ninety-five percent (n = 78/82) considered radiation exposure as problematic in CT examinations, especially in repeat CTs. CONCLUSION: Most final-year medical students were familiar with the sepsis criteria. Still, some referred to outdated diagnostic criteria. Participants saw the ability to plan further patient management based on CT as a major benefit. Most participants were aware of radiation as a risk of CT. CRITICAL RELEVANCE STATEMENT: More detailed knowledge of CT in septic patients should be implemented in the medical curriculum. Retraining of medical students could help increase student confidence potentially improving patient care. KEY POINTS: 1. Whereas the majority of final-year medical students were familiar with sepsis criteria, some referred to outdated diagnostic criteria. 2. Participants saw the ability to plan further patient management based on CT as a major benefit. 3. Most participants were aware of radiation as a risk of CT.

Zinc-Doped Iron Oxide Nanoparticles as a Proton-Activatable Agent for Dose Range Verification in Proton Therapy.

Proton therapy allows the treatment of specific areas and avoids the surrounding tissues. However, this technique has uncertainties in terms of the distal dose fall-off. A promising approach to studying the proton range is the use of nanoparticles as proton-activatable agents that produce detectable signals. For this, we developed an iron oxide nanoparticle doped with Zn (IONP@Zn-cit) with a hydrodynamic size of 10 nm and stability in serum. Cytotoxicity, defined as half of the surveillance, was 100 µg Zn/mL in the U251 cell line. The effect on clonogenic cell death was tested after X-ray irradiation, which suggested a radioprotective effect of these nanoparticles at low concentrations (1-10 µg Zn/mL). To evaluate the production of positron emitters and prompt-gamma signals, IONP@Zn-cit was irradiated with protons, obtaining prompt-gamma signals at the lowest measured concentration (10 mg Zn/mL). Finally, 67Ga-IONP@Zn-cit showed accumulation in the liver and spleen and an accumulation in the tumor tissue of 0.95% ID/g in a mouse model of U251 cells. These results suggest the possibility of using Zn nanoparticles as proton-activatable agents to verify the range by prompt gamma detection and face the challenges of prompt gamma detection in a specific biological situation, opening different avenues to go forward in this field.

Comparison of APIStrip passive sampling with conventional sample techniques for the control of acaricide residues in honey bee hives.

Western honey bees are very sensitive bioindicators for studying environmental conditions, hence frequently included in many investigations. However, it is very common in both research studies and health surveillance programs to sample different components of the colony, including adult bees, brood and their food reserves. These practices are undoubtedly aggressive for the colony as a whole, and may affect its normal functioning and even compromise its viability. APIStrip-based passive sampling allows long-term monitoring of residues without affecting the colony in any way. In this study, we compared the effectiveness in the control of acaricide residues by using passive and conventional sampling, where the residue levels of the acaricides coumaphos, tau-fluvalinate and amitraz were evaluated. Conventional and APIStrip-based sampling differ in methods for evaluating bee exposure to residues. APIStrip is less invasive than conventional sampling, offers more efficient measurement of environmental contaminants, and can be stored at room temperature, saving costs and minimizing operator error.

When should we involve interventional radiology in the management of acute pulmonary embolism?

Pulmonary embolism (PE) is a common disease associated with high morbidity and mortality. Currently, guidelines recommend systemic thrombolysis in patients with haemodynamic instability (high-risk PE) or patients with intermediate-high-risk PE with haemodynamic deterioration. Nevertheless, more than half of high-risk PE patients do not receive systemic thrombolysis due to a perceived increased risk of bleeding. In these cases, percutaneous catheter-directed therapy (CDT) or surgical embolectomy should be considered. CDT has emerged and appears to be an effective alternative in treating PE, with a hypothetical lower risk of bleeding than systemic thrombolysis, acting directly in the thrombus with a much lower dose of thrombolytic drug or even without thrombolytic therapy. CDT techniques include catheter-directed clot aspiration or fragmentation, mechanical embolectomy, local thrombolysis, and combined pharmaco-mechanical approaches. A few observational prospective studies have demonstrated that CDT improves right ventricular function with a low rate of haemorrhage. Nevertheless, the evidence from randomised controlled trials is scarce. Here we review different scenarios where CDT may be useful and trials ongoing in this field. These results may change the upcoming guidelines for management and treatment of PE, establishing CDT as a recommended treatment in patients with acute intermediate-high-risk PE.

Quantitative, Spectro-kinetic Analysis of Oxygen in Electron-Beam Sensitive, Multimetallic Oxide Nanostructures.

The oxygen stoichiometry of hollandite, KxMnO2-δ, nanorods has been accurately determined from a quantitative analysis of scanning-transmission electron microscopy (STEM) X-Ray Energy Dispersive Spectroscopy (XEDS) experiments carried out in chrono-spectroscopy mode. A methodology combining 3D reconstructions of high-angle annular dark field electron tomography experiments, using compressed-sensing algorithms, and quantification through the so-called ζ-factors method of XEDS spectra recorded on a high-sensitivity detector has been devised to determine the time evolution of the oxygen content of nanostructures of electron-beam sensitive oxides. Kinetic modeling of O-stoichiometry data provided K0.13MnO1.98 as overall composition for nanorods of the hollandite. The quantitative agreement, within a 1% mol error, observed with results obtained by macroscopic techniques (temperature-programmed reduction and neutron diffraction) validate the proposed methodology for the quantitative analysis, at the nanoscale, of light elements, as it is the case of oxygen, in the presence of heavy ones (K, Mn) in the highly compromised case of nanostructured materials which are prone to electron-beam reduction. Moreover, quantitative comparison of oxygen evolution data measured at macroscopic and nanoscopic levels allowed us to rationalize beam damage effects in structural terms and clarify the exact nature of the different steps involved in the reduction of these oxides with hydrogen.