RESUMEN
Redox mediators (RMs) are widely utilized in the electrolytes of Li-O2 batteries to catalyze the formation/decomposition of Li2O2, which significantly enhances the cycling performance and reduces the charge overpotential. However, RMs have a shuttle effect by migrating to the Li anode side and inducing Li metal degradation through a parasitic reaction. Herein, a metal-organic framework gel (MOF-gel) separator is proposed to restrain the shuttling of RMs. Compared to traditional MOF nanoparticles, MOF gels form uniform and dense films on the separators. When using Ru(acac)3 (ruthenium acetylacetonate) as an RM, the MOF-gel separator suppresses the shuttling of Ru(acac)3 toward the Li anode side and significantly enhances the performance of Li-O2 batteries. Specifically, Li-O2 batteries exhibit an ultralong cycling life (410 cycles) at a current density of 0.5 A g-1. Moreover, the batteries using the MOF-gel/celgard separator exhibit significantly improved cycling performance (increase by ≈1.6 times) at a high current density of 1.0 A g-1 and a decreased charge/discharge overpotential. This result is expected to guide future development of battery separators and the exploration of redox mediators.
RESUMEN
BACKGROUND: VS-505 (AP301), an acacia and ferric oxyhydroxide polymer, is a novel fiber-iron-based phosphate binder. This two-part Phase 2 study evaluated the tolerability, safety and efficacy of oral VS-505 administered three times daily with meals in treating hyperphosphatemia in chronic kidney disease (CKD) patients receiving maintenance hemodialysis (MHD). METHODS: In Part 1, patients received dose-escalated treatment with VS-505 2.25, 4.50 and 9.00 g/day for 2 weeks each, guided by serum phosphorus levels. In Part 2, patients received randomized, open-label, fixed-dosage treatment with VS-505 (1.50, 2.25, 4.50 or 6.75 g/day) or sevelamer carbonate 4.80 g/day for 6 weeks. The primary efficacy endpoint was the change in serum phosphorus. RESULTS: The study enrolled 158 patients (Part 1: 25; Part 2: 133), with 130 exposed to VS-505 in total. VS-505 was well tolerated. The most common adverse events were gastrointestinal disorders, mainly feces discolored (56%) and diarrhea (15%; generally during Weeks 1-2 of treatment). Most gastrointestinal disorders resolved without intervention, and none was serious. In Part 1, serum phosphorus significantly improved (mean change -2.0 mg/dL; 95% confidence interval -2.7, -1.4) after VS-505 dose escalation. In Part 2, serum phosphorus significantly and dose-dependently improved in all VS-505 arms, with clinically meaningful reductions with VS-505 4.50 and 6.75 g/day, and sevelamer carbonate 4.80 g/day [mean change -1.6 (-2.2, -1.0), -1.8 (-2.4, -1.2) and -1.4 (-2.2, -0.5) mg/dL, respectively]. In both parts, serum phosphorus reductions occurred within 1 week of VS-505 initiation, returning to baseline within 2 weeks of VS-505 discontinuation. CONCLUSION: VS-505, a novel phosphate binder, was well tolerated with a manageable safety profile, and effectively and dose-dependently reduced serum phosphorus in CKD patients with hyperphosphatemia receiving MHD. CLINICAL TRIAL REGISTRATION NUMBER: NCT04551300 .
Asunto(s)
Quelantes , Hiperfosfatemia , Diálisis Renal , Humanos , Masculino , Diálisis Renal/efectos adversos , Femenino , Persona de Mediana Edad , Hiperfosfatemia/tratamiento farmacológico , Hiperfosfatemia/etiología , Anciano , Quelantes/administración & dosificación , Quelantes/uso terapéutico , Quelantes/efectos adversos , Relación Dosis-Respuesta a Droga , Adulto , Fosfatos/sangre , Compuestos Férricos/administración & dosificación , Compuestos Férricos/efectos adversos , Compuestos Férricos/uso terapéutico , Sevelamer/administración & dosificación , Sevelamer/uso terapéutico , Estudios de Seguimiento , Fallo Renal Crónico/terapia , Fallo Renal Crónico/complicaciones , Insuficiencia Renal Crónica/terapia , Insuficiencia Renal Crónica/complicacionesRESUMEN
BACKGROUND: To access the efficacy of percutaneous transluminal angioplasty and arteriovenous fistula reconstruction for immature arteriovenous fistula, compare the long-term patency and post-operative complications between them. MATERIALS AND METHODS: The medical records and Hemodialysis record sheets from 44 patients between May 2020 and January 2022 who underwent percutaneous transluminal angioplasty or arteriovenous fistula reconstruction treatment for immature autogenous arteriovenous fistula (AVF) were retrospectively reviewed. The patients were divided into two groups according to the type of surgery they received, including 25 patients in the PTA group and 19 patients in the AVF reconstruction group. Clinical outcomes were included, such as the primary and secondary patency rates following the procedure, maturation time, peak systolic velocity (PSV) of brachial artery, maximum pump-controlled blood flow at initial dialysis, and post-operative complications rates in the two groups. RESULTS: Technical and clinical success was achieved in 100% of the 44 cases. For patients who underwent percutaneous transluminal angioplasty, the primary patency rate at 3, 6, and 9 months was 84.0%, 68.0%, 60.0%, and the secondary patency rate was 92.0%, 84.0%, 80.0%, respectively. And for patients who underwent arteriovenous fistula reconstruction, the primary patency rate at 3, 6, and 9 months was 89.5%, 73.7%, 68.4%, and the secondary patency rate was 100.0%, 94.7%, 94.7%, respectively. There were no significant differences between the two groups in terms of patency rates (p > .050). In patients whose maturation was successful, the average maturation time of fistula after the PTA procedure was 19.36 ± 13.94 days, and 58.63 ± 18.95 days for the reconstruction procedure (p < .010). The PSV of brachial artery before and after the procedure was 87.64 ± 23.87 cm/s and 153.20 ± 21.69 cm/s in PTA group, for reconstruction group, the number was 86.26 ± 20.59 cm/s and 151.26 ± 29.94 cm/s, respectively. No statistically significant differences (p > .050). The maximum pump-controlled blood flow at initial dialysis was 232.60 ± 16.72 ml/min in PTA group, which was significantly higher than 197.11 ± 10.45 ml/min in reconstruction group (p < .010). Subcutaneous hematoma, restenosis, thrombus formation, and pseudoaneurysm were major complications in PTA group. Restenosis, thrombus formation, and pseudoaneurysm were major complications in reconstruction group, with no statistically significant differences between the two groups (p > .050). CONCLUSION: When immature AVFs require reconstruction surgery, the patency outcomes are comparable to AVFs that undergo successful management by PTA. While, when AVFs are successfully managed by PTA, they have significantly less maturation times and higher maximum pump-controlled blood flow rates at initial dialysis AVF use.
Asunto(s)
Aneurisma Falso , Fístula Arteriovenosa , Derivación Arteriovenosa Quirúrgica , Trombosis , Humanos , Oclusión de Injerto Vascular/etiología , Oclusión de Injerto Vascular/terapia , Grado de Desobstrucción Vascular/fisiología , Estudios Retrospectivos , Aneurisma Falso/complicaciones , Diálisis Renal/efectos adversos , Angioplastia/efectos adversos , Angioplastia/métodos , Fístula Arteriovenosa/complicaciones , Derivación Arteriovenosa Quirúrgica/efectos adversos , Constricción Patológica , Resultado del TratamientoRESUMEN
Hierarchical carbon nanocages as emerging nanomaterials have a great potential for photothermal therapy due to their unique porous structure, high specific surface area, and excellent photothermal property. Herein, a hierarchical nitrogen-doped carbon nanocage (hNCNC) is introduced as a second near-infrared photothermal agent, and then functionalizes it with metal-organic hydrogel (MOG) to form a thermal-responsive switch for sensitized photothermal therapy. Upon 1064 nm light irradiation, the hNCNCs exhibit a remarkable photothermal conversion efficiency of 65.9% owing to a high near-infrared extinction coefficient. Meanwhile, due to the hierarchical structure, hNCNCs show 60.2% (wt./wt.) loading efficiency of quercetin, a heat shock protein (Hsp70) inhibitor. Through thermal-driven dry-gel transformation, the coating MOGs intelligently release the encapsulated quercetin for sensitizing cancer cells to heat. Based on the synergistic effect of hyperthermia elevation and thermal-driven drug release, the dual thermal utilization platform achieves effective photothermal tumor ablation in vivo under low concentration of hNCNCs and mild irradiation, which provides a new diagram of intelligent responsive photothermal agents for enhanced photothermal therapy.
Asunto(s)
Carbono , Hipertermia Inducida , Carbono/química , Fototerapia , Terapia Fototérmica , Línea Celular Tumoral , Hidrogeles/farmacología , Hidrogeles/química , Quercetina/farmacología , Metales , Doxorrubicina/farmacologíaRESUMEN
This work investigates a self-masking technology for roughening the surface of light-emitting diodes (LEDs). The carbonized photoresist with a naturally nano/micro-textured rough surface was used as a mask layer. After growing the Si3N4 passivation layer on LEDs, the texture pattern of the mask layer was transferred to the surface of the passivation layer via reactive ion beam (RIE) dry etching, resulting in LEDs with nano-textured surfaces. This nano-textured surface achieved by self-masking technology can alleviate the total internal reflection at the top interface and enhance light scattering, thereby improving the light extraction efficiency. As a result, the wall-plug efficiency (WPE) and external quantum efficiency (EQE) of rough-surface LEDs reached 53.9% and 58.8% at 60 mA, respectively, which were improved by 10.3% and 10.5% compared to that of the flat-surface Si3N4-passivated LED. Additionally, at the same peak, both LEDs emit a wavelength of 451 nm at 350 mA. There is also almost no difference between the I-V characteristics of LEDs before and after roughening. The proposed self-masking surface roughening technology provides a strategy for LEE enhancement that is both cost-effective and compatible with conventional fabrication processes.
RESUMEN
As a newly discovered way of cell death, pyroptosis has been gradually discovered in acute and chronic kidney disease. Existing studies have shown that reactive oxygen species (ROS) can induce pyroptosis and release a large number of inflammatory mediators, resulting in kidney damage. As a transcription factor, transcription factor EB(TFEB) can regulate mitochondrial energy metabolism, reduce the production of ROS, and reduce the inflammatory damage of vascular endothelial cells. In a high-glucose environment, whether TFEB can regulate oxidative stress in HK-2 cells, thereby reducing pyroptosis, has not yet been studied. This study found that in HK-2 cells, with the prolongation of high concentration glucose stimulation, the expression level of TFEB showed a trend of first increasing and then decreasing; and nuclear translocation of TFEB expression occurred within 24 h. In high-glucose environment, the expression of pyroptosis-related proteins gradually increased over time, while the expression of anti-oxidative stress proteins superoxide dismutase2(SOD2)and NAD(P)H: quinone oxidoreductase 1(NQO1) showed a trend of first increasing and then decreasing. After TFEB was transfected with overexpression plasmid, the expression levels of SOD2 and NQO1 increased significantly, and the expression of pyroptosis-related proteins decreased. Observed under a confocal microscope after Mitosox red staining, the expression of ROS in the TFEB overexpression group decreased. After down-regulating the expression of TFEB, the expression of ROS increased. The research results suggested that in HK-2 cells in the high glucose environment, TFEB may affect the pyroptosis by regulating the expression of antioxidant enzymes SOD2 and NQO1, which provides a new therapeutic idea for the treatment of diabetic nephropathy.
Asunto(s)
Células Endoteliales , Piroptosis , Células Endoteliales/metabolismo , Glucosa/metabolismo , Glucosa/farmacología , NAD/metabolismo , Estrés Oxidativo , Especies Reactivas de Oxígeno/metabolismoRESUMEN
Oxidative stress-induced cellular senescence and inflammation are important biological events in diabetic nephropathy (DN). Our recent studies have found that pyrroloquinoline quinine (PQQ) has protective effects against HG-induced oxidative stress damage and apoptosis in HK-2 cells. Nevertheless, whether PPQ has the effect of anti-inflammation and anti-senescence in HK-2 cells remains unclear. Here, we showed that low-dose PPQ treatment (100â¯nM) downregulates the expression of P16, P21, IL-1ß, TNF-α and NF-κB in HG cultured HK-2 cells. A low dose of PPQ also upregulated the protein expression of SOD2, CAT and inhibited the generation of ROS. We also indicated that PPQ affected the activity of Keap1/Nrf2 pathway, increased the nuclear accumulation of Nrf2 and the downstream pathway protein expression of Keap1/Nrf2 signaling pathway (HO-1, NQO-1, GST and GPx-3). When ML385 was added to inhibit the activity of Keap1/Nrf2 signaling pathway, the effects of PPQ on anti-oxidative stress, anti-inflammation and anti-senescence in HK-2 cells under HG condition were weakened. In conclusion, our results suggest that PPQ could modulate HG-induced inflammation and senescence in HK-2 cells via the inhibition of ROS generation and achieves the protective effects through Keap1/Nrf2 pathway and upregulating the expression of its target protein.
Asunto(s)
Antiinflamatorios/farmacología , Antioxidantes/farmacología , Células Epiteliales/efectos de los fármacos , Proteína 1 Asociada A ECH Tipo Kelch/metabolismo , Riñón/citología , Factor 2 Relacionado con NF-E2/metabolismo , Pirroles/farmacología , Quinolinas/farmacología , Línea Celular , Senescencia Celular/efectos de los fármacos , Células Epiteliales/metabolismo , Humanos , Estrés Oxidativo/efectos de los fármacos , Transducción de Señal/efectos de los fármacosRESUMEN
High glucose(HG)-induced oxidative stress and apoptosis in renal tubular epithelial cells play an important role in the pathogenesis of diabetic nephropathy. Pyrroloquinoline quinine (PQQ), a new B vitamin, has been demonstrated to be important in antioxidant and anti-apoptotic effects. However, its effect on HK-2â¯cells and the potential mechanism are rarely investigated. In this study, we investigated that PPQ had protective effects against HG-induced oxidative stress damage and apoptosis in vitro model of diabetic nephropathy. PPQ at 10, 100, 500, 1000 and 10000â¯nM could protect HK-2â¯cell from HG-induced inhibition. The protective effects of PQQ were associated with increasing the level of antioxidants(SOD2, CAT), inhibition of reactive oxygen species(ROS) production, and dependent modulation of Bcl-2 family proteins. PPQ significantly upregulated the protein and mRNA expression of Sirtuin3(Sirt3) in HG-induced HK-2â¯cells. PPQ also reduced apoptosis in HG-induced HK-2â¯cells by the PI3K/Akt/FoxO3a signal pathway. As down-regulated sirt3 or inhibitory the activity of PI3K/Akt/FoxO3a pathway, the protective effects of PPQ were weakened. In conclusion, our data suggest that PPQ achieves the protective effects through PI3K/Akt/FoxO3a pathway and dependent modulation of Sirt3.
Asunto(s)
Riñón/efectos de los fármacos , Riñón/metabolismo , Cofactor PQQ/farmacología , Apoptosis/efectos de los fármacos , Línea Celular , Nefropatías Diabéticas/metabolismo , Nefropatías Diabéticas/patología , Nefropatías Diabéticas/prevención & control , Proteína Forkhead Box O3/metabolismo , Glucosa/metabolismo , Humanos , Riñón/patología , Modelos Biológicos , Estrés Oxidativo/efectos de los fármacos , Fosfatidilinositol 3-Quinasas/metabolismo , Sustancias Protectoras/farmacología , Proteínas Proto-Oncogénicas c-akt/metabolismo , Transducción de Señal/efectos de los fármacos , Sirtuina 3/metabolismoRESUMEN
Paclitaxel is a widely used chemotherapy drug for advanced laryngeal cancer patients. However, the fact that there are 20-40% of advanced laryngeal cancer patients do not response to paclitaxel makes it necessary to figure out potential biomarkers for paclitaxel sensitivity prediction. In this work, Hep2, a laryngeal cancer cell line, untreated or treated with lower dose of paclitaxel for 24 h, was applied to DNA microarray chips for gene and miR expression profile analysis. Expression of eight genes altered significantly following paclitaxel treatment, which was further validated by quantitative real-time PCR. Four up-regulated genes were ID2, BMP4, CCL4 and ACTG2, in which ID2 and BMP4 were implicated to be involved in several drugs sensitivity. While the down-regulated four genes, MAPK4, FASN, INSIG1 and SCD, were mainly linked to the endoplasmic reticulum and fatty acid biosynthesis, these two cell processes that are associated with drug sensitivity by increasing evidences. After paclitaxel treatment, expression of 49 miRs was significantly altered. Within these miRs, the most markedly expression-changed were miR-31-star, miR-1264, miR-3150b-5p and miR-210. While the miRs putatively modulated the mRNA expression of the most significantly expression-altered genes were miR-1264, miR-130a, miR-27b, miR-195, miR-1291, miR-214, miR-1277 and miR-1265, which were obtained by miR target prediction and miRNA target correlation. Collectively, our study might provide potential biomarkers for paclitaxel sensitivity prediction and drug resistance targets in laryngeal cancer patients.
Asunto(s)
Antineoplásicos Fitogénicos/farmacología , Biomarcadores de Tumor/genética , Resistencia a Antineoplásicos/genética , Perfilación de la Expresión Génica , Neoplasias Laríngeas/genética , MicroARNs/metabolismo , Paclitaxel/farmacología , Línea Celular Tumoral , Supervivencia Celular/efectos de los fármacos , Relación Dosis-Respuesta a Droga , Perfilación de la Expresión Génica/métodos , Regulación Neoplásica de la Expresión Génica , Humanos , Concentración 50 Inhibidora , Neoplasias Laríngeas/patología , Análisis de Secuencia por Matrices de Oligonucleótidos , Reacción en Cadena en Tiempo Real de la Polimerasa , Factores de TiempoRESUMEN
BACKGROUND: Diabetic nephropathy is a complex disease with poor outcomes, and our current treatment measures are limited. It is urgent to search for novel therapeutic targets. Recently, a mesangium-predominant gene, megsin, has emerged as a participant in mesangial cell proliferation and/or mesangial matrix expansion. This study investigated the effect of megsin down-regulation on the progression of diabetic nephropathy. METHODS: Streptozotocin (STZ)-induced diabetic CD-1 mice after uninephrectomy received a pBAsi mU6 Neo megsin siRNA plasmid for 12 weeks and were compared with age-matched nondiabetic mice. In vitro mouse mesangial cells were transfected with pBAsi mU6 Neo megsin siRNA plasmid using Lipofectamine 2000 reagent and further cultured in DMEM containing high glucose for up to 48 hours. All of the cells were collected for protein extraction and the supernatant for type IV collagen measurement. The expression of megsin, matrix metalloproteinase-2 (MMP-2), tissue inhibitor of metalloproteases-2 (TIMP-2) and p27(Kip1) was determined by Western blotting. RESULTS: The megsin siRNA plasmid alleviated proteinuria and glomerular type IV collagen accumulation 12 weeks after the STZ injection, down-regulated renal cell proliferation and normalized the imbalance between MMP-2 and TIMP-2. Also, in vitro experiments showed that the glomerular mesangial cellular proliferation and type IV collagen production induced by high glucose were relieved after the transfection of megsin siRNA plasmid. The level of p27(kip1) was down-regulated in transfected mesangial cells significantly. CONCLUSIONS: The study suggests that the down-regulation of megsin might exert beneficial effects on the diabetic kidney partly through down-regulation of p27(kip1) level and that megsin may serve as a novel therapeutic target in the management of diabetic nephropathy.
Asunto(s)
Inhibidor p27 de las Quinasas Dependientes de la Ciclina/metabolismo , Diabetes Mellitus Experimental/terapia , Nefropatías Diabéticas/prevención & control , Terapia Genética/métodos , Células Mesangiales/metabolismo , Interferencia de ARN , ARN Interferente Pequeño/metabolismo , Serpinas/genética , Animales , Western Blotting , Proliferación Celular , Células Cultivadas , Colágeno Tipo IV/metabolismo , Creatinina/sangre , Diabetes Mellitus Experimental/complicaciones , Diabetes Mellitus Experimental/genética , Diabetes Mellitus Experimental/metabolismo , Diabetes Mellitus Experimental/patología , Nefropatías Diabéticas/etiología , Nefropatías Diabéticas/genética , Nefropatías Diabéticas/metabolismo , Nefropatías Diabéticas/patología , Regulación hacia Abajo , Masculino , Metaloproteinasa 2 de la Matriz/metabolismo , Células Mesangiales/patología , Ratones , Nefrectomía , Proteinuria/etiología , Proteinuria/genética , Proteinuria/metabolismo , Proteinuria/prevención & control , ARN Interferente Pequeño/administración & dosificación , Serpinas/metabolismo , Factores de Tiempo , Inhibidor Tisular de Metaloproteinasa-2/metabolismo , TransfecciónRESUMEN
Simultaneous full scan-selected ion monitoring mode (Scan-SIM) is a new improvement method of data acquisition of gas chromatography-mass spectrometry (GC-MS). A method of determing alkaloids in tobacco was established by GC-MS with Scan-SIM. Nicotine, nornicotine, anabasine and anatabine were determined with scan mode, and myosmine, nicotyrine, 2,3'-bipyridyl and cotinine were determined with SIM mode. The average recoveries of alkaloids ranged from 94.8% to 98.8%, and the relative standard deviations were less than 6.0% (n = 5). Therefore, it is a simple, rapid, accurate method. Tobacco samples picked in different years were determined using this method, and the results were satisfactory.
Asunto(s)
Alcaloides/análisis , Cromatografía de Gases y Espectrometría de Masas/métodos , Nicotiana/química , Calibración , Modelos Lineales , Reproducibilidad de los Resultados , Solventes/química , Factores de TiempoRESUMEN
A method for simultaneous determination of seven nonvolatile organic acids (NVOAs), five semivolatile organic acids (SVOAs), and twelve volatile organic acids (VOAs) in tobacco by synchronous SIM (Selected Ion Monitoring)-scan mode GC-MS was developed. The collection of NVOAs and SVOAs data was performed in full-scan mode, and that of VOAs data was carried out with SIM. Recoveries of NVOAs and SVOAs varied from 90.0 to 103.0%, and RSDs were less than 4.0%; recoveries of VOAs ranged from 89.5 to 99.3%, and their RSDs were less than 3.0%. Twelve tobacco samples were analyzed by the described method, and the results show that the method is applicable for the simultaneous determination of VOAs, NVOAs, and SVOAs in tobacco.
Asunto(s)
Ácidos Carboxílicos/análisis , Ácidos Grasos/análisis , Cromatografía de Gases y Espectrometría de Masas , Nicotiana/química , Ácidos Carboxílicos/química , Ácidos Grasos/química , Reproducibilidad de los Resultados , VolatilizaciónRESUMEN
A fast method for determination of polycyclic aromatic hydrocarbons (PAHs) in water samples was established. The samples from the Dianchi Lake and Panlong River were analyzed directly using stir bar sorptive extraction-thermal desorption system-gas chromatography/ mass spectrometry (SBSE-TDS-GC/MS). Polydimethylsiloxane (PDMS) was used as the extraction phase. The samples were extracted with stir bars at 1100 r/min for 60 min at ambient temperature (25 degrees C). Desorption was carried out at 300 degrees C for 5 min under a helium flow of 50 mL/min in the splitless mode while maintaining a cryofocusing temperature of 0 degrees C in the programmed-temperature vaporization (PTV) injector of the GC/MS system. The limits of detection of PAHs ranged from 1.0 pg to 468.8 pg. The theoretical recoveries of PAHs were greater than 90% (except that naphthalene was 64.90%), and the recoveries of 16 PAHs from water samples ranged from 83.1% to 109.4%, and the relative standard deviations (RSDs) ranged from 1.2% to 9.3% (n = 6). PAHs in Dianchi Lake and Panlong River samples were quantified rapidly by this method. The results show that, the total content of these 16 PAHs is 89.16 ng/L in Dianchi Lake, 65.41 ng/L in the up-stream of Panlong River, 339.22 ng/L in the middle-stream of Panlong River and 62.25 ng/L in the down-stream of Panlong River. It is demonstrated that the Dianchi Lake and Panlong River were polluted by PAHs to some degree.
RESUMEN
A novel method for the determination of 5 pyrethroid pesticide residues in tobacco leaf and tea samples was established. The pesticide residues in the samples were extracted and concentrated with stir bar, desorbed by thermal desorption system, and then determined by gas chromatography-mass spectrometry (GC-MS). The pesticide residues in the samples were extracted with a stir bar at 1 100 r/min for 1 h. The desorption was carried out at 300 degrees C for 4 min under a helium flow of 50 mL/min while maintaining a cryofocusing temperature of 0 degrees C in the CIS-4 injector of the GC-MS system. Finally, the CIS-4 injector was raised to a temperature of 300 degrees C and then the analytes were separated by GC and detected by MS. The limits of detection of this method for the tobacco leaves ranged from 3.3 ng to 11.4 ng. The recoveries of pesticides from the tobacco leaves ranged from 94.8% to 103.4% and the relative standard deviations (RSDs) of peak areas ranged from 5.3% to 8.6% (n = 6). The limits of detection of this method for tea ranged from 4.2 ng to 10.5 ng. The recoveries of pesticides from tea ranged from 98.2% to 110.1% and the RSDs of peak areas were less than 9.6% (n = 6). Therefore, this method can satisfy the requirements for the rapid analysis of pesticide residues in the tobacco leaf and tea samples.
Asunto(s)
Cromatografía de Gases y Espectrometría de Masas/métodos , Nicotiana/química , Residuos de Plaguicidas/análisis , Hojas de la Planta/química , Piretrinas/análisis , Té/química , Cloruro de Sodio/químicaRESUMEN
A novel method for the analysis of chemical components in tobacco flavors was established using stir bar sorptive extraction (SBSE) and thermal desorption coupled with gas chromatography-mass spectrometry (GC-MS). The different parameters affecting the extraction of the analytes from the samples to the poly (dimethylsiloxane) (PDMS) coated stir bars and the conditions affected thermal desorption were investigated. The optimized extraction conditions were that the sample was extracted with a stir bar (10 mm length and 0.5 mm thickness) at 1 100 r/min for 1 h at ambient temperature. Desorption was carried out from 20 degrees C ramped to 250 degrees C at 60 degrees C/min and hold for 2 min under a helium flow of 50 mL/min in the splitless mode while maintained the cryofocusing temperature of - 100 degrees C in a CIS-4 injector of the GC-MS system. Finally, the CIS-4 injector was raised to a temperature of 280 degrees C and the analytes were separated by GC and detected by MS using full scan mode (m/z 35 - 400). Under the described conditions, about 30 components were identified from the tobacco flavors, and the major components included esters, ketones, aldehydes, etc. The average relative standard deviation (RSD) of peak areas of 30 components for 6 determinations was less than 10%. The good repeatability made SBSE a powerful tool for the routine quality control analysis of chemical components in tobacco flavors.
RESUMEN
To further understand the effect of tobacco stems in tobacco blend, a detailed comparative study of chemical components of tobacco leaves and stems before and after combustion was carried out. Pyrolysis of tobacco leaves and stems was carried out by a CDS Pyrolyser 2000 coupled to a Finnigan 8000(TOP) Gas Chromatograph and a Voyager Mass Spectrometer (GC-MS). A modified apparatus of pyrolysis was used to emulate the behavior of combustion of cigarette. A set of pyrolysis conditions was also developed that approximated those occurring in the pyrolysis region of the burning cigarette. The conditions included heating the sample at 20 degrees C/ms from 30 degrees C to 300 degrees C, 600 degrees C and 900 degrees C in air, and their pyrolysates were analyzed by GC-MS. The results indicated that the values of routine chemical constituents in tobacco leaves and stems were obviously different. The pyrolysates belonged to numerous classes of compounds such as hydrocarbons, alcohols, phenols, aldehydes, ketones, nitriles, alkaloids etc. The kinds of pyrolysates of tobacco leaves and stems were positively related to the pyrolysis temperature levels. On the other hand, at the same temperature level, the types of the pyrolysates from the tobacco leaves were much more than those from the tobacco stems.
Asunto(s)
Nicotiana/química , Fenómenos Químicos , Cromatografía de Gases y Espectrometría de Masas , Calor , Hojas de la Planta/química , Tallos de la Planta/químicaRESUMEN
Relationships between tobacco compounds and smoke products are complex and often difficult to unravel. Pyrolysis experiments have frequently been used to establish such relationships. The relevance of pyrolysis experiments to the behavior of tobacco constituent in a burning cigarette was studied. A set of pyrolysis conditions has been developed to study the effect of thermal degradation of beta-carotene to the cigarette smoke quality, and the conditions was approximated to those occurring in the pyrolysis region of the burning cigarette. The pyrolysates of beta-carotene were investigated in air, 10% O2 (in N2) and N2 at three temperature levels of 300 degrees C, 600 degrees C and 900 degrees C, respectively. The pyrolysates were adsorbed by solid-phase microextraction (SPME) and then analyzed by gas chromatography/mass spectrometry (GC/ MS). Under the different conditions, the major pyrolysates from beta-carotene are hydrocarbon compounds such as toluene, p-xylene, 1, 2, 3, 4-tetrahydro-1, 1, 6-trimethyl-naphthalene and 2, 7-dimethyl-naphthalene, and some important flavors existing in cigarette smoke such as isophorone, 2, 6, 6-trimethyl-1-cyclohexene-1-carboxaldehyde, beta-ionone and 5, 6, 7, 7a-tetrahydro-4, 4, 7 a-trimethyl-2 (4H)-benzofuranone. The amount of these pyrolysates alters with the change of pyrolysis temperature levels and the concentration of oxygen.
Asunto(s)
Nicotiana/química , beta Caroteno/química , Fenómenos Químicos , Cromatografía de Gases y Espectrometría de Masas , Calor , Humo , Microextracción en Fase SólidaRESUMEN
2-(2-Quinolinylazo)-5-dimethylaminobenzoic acid (QADMAB) is proposed as a new sensitive and selective chromogenic reagent for spectrophotometric determination of cobalt. The QADMAB reacts with cobalt in the presence of cetyl trimethylammonium bromide (CTMAB) medium to form a violet complex of molar ratio 1:2 (cobalt to QADMAB) in the pH range 3.2-5.2. The molar absorptivity of the complex is 1.28x10(5) L mol(-1) cm(-1) at 625 nm. Beer's law is obeyed in range 0.01-0.32 micro g mL(-1). The relative standard deviation for eleven replicate samples of 0.2 micro g mL(-1) is 0.76%. This method was applied to the determination of cobalt in biological samples, Vitamin B(12), alloys and water with good results.
Asunto(s)
Benzoatos/química , Compuestos Cromogénicos/química , Cobalto/análisis , Quinolinas/química , Espectrofotometría/métodos , Cabello/química , Humanos , Concentración de Iones de Hidrógeno , Sensibilidad y Especificidad , Té/química , Nicotiana/química , Vitamina B 12/química , Contaminantes Químicos del Agua/análisis , ortoaminobenzoatosRESUMEN
This paper reports the utilization of solid-phase extraction and the reversed-phase high-performance liquid chromatography for the determination of six important transition metal ions: iron, cobalt, nickel, copper, zinc and manganese in tobacco with 2-(2-quinolinylazo)-5-dimethylaminophenol (QADMAP) as chelating reagent. Iron, cobalt, nickel, copper, zinc and manganese ions react with QADMAP to form colored chelates in the medium of acetic acid-sodium acetate buffer solution (pH 4.0). These chelates can be enriched by solid-phase extraction with Waters Sep-Pak-C18 cartridge, and eluted the retained chelates from cartridge with tetrahydrofuran. The chelates were separated on a Waters Nova-Pak-C18 column (150x3.9 mm, 5 microm) by gradient elution with methanol (containing 0.5% of acetic acid) and 0.05 mol/l pH 4.0 acetic acid-sodium acetate buffer solution as mobile phase at a flow-rate of 0.5 ml/min. The detection limits of iron, cobalt, nickel, copper, zinc and manganese are 10, 12, 8, 13, 17 and 22 ng/l, respectively. This method had been applied to the determination of iron, cobalt, nickel, copper, zinc and manganese in tobacco with good results.