RESUMO
A 3D-printed microfluidic tool for assessing local drug delivery systems (LDD) in simulated in vivo conditions was developed and evaluated. The device was designed considering the oral environment and dental applications, and it was fabricated with a high-precision resin 3D printer. Chitosan scaffolds loaded with different concentrations of doxycycline were used for evaluating our device. The concentration of the released drug was measured through in-line UV-VIS spectroscopy, and to verify the repeatability and accuracy of our measurements, comparisons with standard HPLC results were made (5% deviation). Cumulative drug release profiles in steady-state conditions were obtained and compared to the Weibull model. The behaviour of the LDD system in a dynamic environment was also evaluated during experiments where step changes in pH were introduced. It was demonstrated that under infection-like conditions, there is an immediate response from the polymer and a clear increase in the concentration of the released drug. Continuous flow and recirculation experiments were also conducted, revealing significant differences in the drug release profiles. Specifically, in the case of continuous flow, the quantity of the released drug is much higher due to the higher driving force for diffusion (concentration gradient). Overall, the proposed microfluidic tool proved to be ideal for evaluating LDD systems, as the in vivo microenvironment can be replicated in a better way than with currently used standard systems.
Assuntos
Quitosana , Doxiciclina , Sistemas de Liberação de Medicamentos , Liberação Controlada de Fármacos , Doxiciclina/administração & dosagem , Doxiciclina/análise , Quitosana/química , Sistemas de Liberação de Medicamentos/instrumentação , Técnicas Analíticas Microfluídicas/instrumentação , Impressão Tridimensional , Dispositivos Lab-On-A-Chip , Desenho de EquipamentoRESUMO
A novel smartphone-assisted fluorescent sensor based on europium/zirconium metal-organic framework (Eu0.5/Zr0.5-MOF) was developed for the fast and sensitive determination of doxycycline (DOX) and L-arginine (Arg). After the addition of DOX, the fluorescence of Eu0.5/Zr0.5-MOF was quenched owing to the inner filter effect (IFE). When Arg was introduced into the Eu0.5/Zr0.5-MOF@DOX complex system, the fluorescence was recovered because the interaction between Arg and Eu0.5/Zr0.5-MOF@DOX weakened the IFE. Moreover, the Eu0.5/Zr0.5-MOF produced continuous fluorescence color changes for the visual measurement of DOX and Arg. The fluorescent probe for DOX and Arg offered broad linear ranges of 0.05-80 and 0.1-60 µg/mL, respectively, with detection limits as low as 2.07 and 67.5 ng/mL. The proposed method was successfully applied to monitor DOX in eggs and Arg in human serum. This work provides a powerful platform for the real-time and visual analysis of DOX and Arg in food and biological samples.
Assuntos
Arginina , Doxiciclina , Corantes Fluorescentes , Smartphone , Arginina/química , Arginina/análise , Doxiciclina/análise , Doxiciclina/química , Corantes Fluorescentes/química , Humanos , Limite de Detecção , Espectrometria de Fluorescência/métodos , Ovos/análise , Animais , Estruturas Metalorgânicas/química , Contaminação de Alimentos/análise , FluorescênciaRESUMO
Sensor array methods have received much attention in recent years. In this study, a colorimetric sensor array consisting of three kinds of steel slag-based composites (including porphyrin-functionalized non-magnetic steel slag (NMSS-Por), alkali-excited steel slag (A-SS), and platinum modified steel slag (ALANH-Pt)) was developed for the detection and recognition of tetracycline antibiotics (TCs) such as tetracycline (TC), oxytetracycline (OTC) and doxycycline (DOX). Linear discriminant analysis (LDA) and hierarchical cluster analysis (HCA) showed that the colorimetric sensor array has excellent recognition ability for TCs. The detection limits of this sensor array for TC, OTC, and DOX were 0.059 µM, 0.111 µM and 0.118 µM, respectively, which provided higher sensitivity compared to the colorimetric sensors composed of a single steel slag-based composite material. At the same time, the array sensor has anti-interference ability, and this study provides a new application route for steel slag.
Assuntos
Antibacterianos , Colorimetria , Aço , Colorimetria/métodos , Colorimetria/instrumentação , Aço/química , Antibacterianos/análise , Limite de Detecção , Tetraciclina/análise , Tetraciclina/química , Tetraciclinas/análise , Doxiciclina/análise , Doxiciclina/química , Análise DiscriminanteRESUMO
Antibiotics are a new type of environmental pollutants. Due to its wide application in many fields, antibiotic residues are ubiquitous in the wastewater environments. Given their potential threat on water ecosystem functioning and public health, the detection of antibiotic residues in wastewater environments has become very necessary. Based on the complexation of Al3+ with flumequine (FLU), ciprofloxacin (CIP) and doxycycline hydrochloride (DOX), their molecular conjugated area were increased and fluorescence intensity were enhanced, combined with synchronous fluorescence spectrometry (SFS) had good selectivity and high sensitivity, a novel method of Al3+ sensitized synchronous fluorescence spectrometry for the determination of FLU, CIP and DOX residues in wastewater was established. When the wavelength difference (Δλ) was selected 115.0 nm, synchronous fluorescence spectra of the three antibiotics could be well separated and the interference of wastewater matrix were eliminated primely. The new SFS made good use of spectral separation instead of conventional chemical separation, and the actual wastewater sample could be directly determined after simple filtration. The experiment results showed that the concentrations of FLU, CIP and DOX in the range of 0.5000-800.0 ng·mL-1, 0.5000-640.0 ng·mL-1 and 10.00-3500 ng·mL-1 had a good linear relationship with fluorescence intensity. The detection limits of three antibiotics were 0.02054 ng·mL-1, 0.03956 ng·mL-1 and 0.8524 ng·mL-1, respectively. Recovery rates of three antibiotics in wastewater samples were 90.72%-98.23%, 88.68%-95.08% and 85.94%-96.70%. The new SFS established in this experiment had the advantages of simple, rapid, sensitive, accurate and good selectivity. Simultaneous and rapid detection of FLU, CIP and DOX residues in wastewater was successfully realized. It had good application prospects in real-time water quality monitoring.
Assuntos
Ciprofloxacina , Doxiciclina , Fluoroquinolonas , Espectrometria de Fluorescência , Águas Residuárias , Poluentes Químicos da Água , Águas Residuárias/química , Ciprofloxacina/análise , Espectrometria de Fluorescência/métodos , Poluentes Químicos da Água/análise , Doxiciclina/análise , Fluoroquinolonas/análise , Antibacterianos/análise , Alumínio/análiseRESUMO
The development of high-performance sensors for doxycycline (DOX) detection is necessary because its residue accumulation will cause serious harm to human health and the environment. Here, a novel tri-emission ratiometric fluorescence sensor was proposed by using "post-mixing" strategy of different emissions fluorescence molecularly imprinted polymers with salicylamide as dummy template (DMIPs). BSA was chosen as assistant functional monomer, and also acted as sensitizers for the aggregation-induced emission (AIE) effect of DOX. The blue-emitting carbon dots and the red-emitting CdTe quantum dots were separately introduced into DMIPs as the response signals. Upon DOX recognition within 2 min, blue and red fluorescence of the tri-emission DMIPs sensor were quenched while green fluorescence of DOX was enhanced, resulting in a wide range of color variations observed over bluish violet-rosered-light pink-orange-yellow-green with a detection limit of 0.061 µM. The sensor possessed highly selective recognition and was successfully applied to detect DOX in complicated real samples. Moreover, with the fluorescent color collection and data processing, the smartphone-assisted visual detection of the sensors showed satisfied sensitivity with low detection limit. This work provides great potential applications for rapid and visual detection of antibiotics in complex substrates.
Assuntos
Antibacterianos , Compostos de Cádmio , Doxiciclina , Impressão Molecular , Pontos Quânticos , Espectrometria de Fluorescência , Telúrio , Doxiciclina/análise , Doxiciclina/química , Pontos Quânticos/química , Telúrio/química , Antibacterianos/análise , Compostos de Cádmio/química , Limite de Detecção , Fluorescência , Carbono/química , Corantes Fluorescentes/química , Polímeros Molecularmente Impressos/química , SmartphoneRESUMO
BACKGROUND: Doxycycline postexposure prophylaxis (PEP) has been shown to prevent sexually transmitted infections (STIs) among cisgender men and transgender women, but data from trials involving cisgender women are lacking. METHODS: We conducted a randomized, open-label trial comparing doxycycline PEP (doxycycline hyclate, 200 mg taken within 72 hours after condomless sex) with standard care among Kenyan women 18 to 30 years of age who were receiving preexposure prophylaxis against human immunodeficiency virus (HIV). The primary end point was any incident infection with Chlamydia trachomatis, Neisseria gonorrhoeae, or Treponema pallidum. Hair samples were collected quarterly for objective assessment of doxycycline use. RESULTS: A total of 449 participants underwent randomization; 224 were assigned to the doxycycline-PEP group and 225 to the standard-care group. Participants were followed quarterly over 12 months. A total of 109 incident STIs occurred (50 in the doxycycline-PEP group [25.1 per 100 person-years] and 59 in the standard-care group [29.0 per 100 person-years]), with no significant between-group difference in incidence (relative risk, 0.88; 95% confidence interval [CI], 0.60 to 1.29; P = 0.51). Among the 109 incident STIs, chlamydia accounted for 85 (78.0%) (35 in the doxycycline-PEP group and 50 in the standard-care group; relative risk, 0.73; 95% CI, 0.47 to 1.13). No serious adverse events were considered by the trial investigators to be related to doxycycline, and there were no incident HIV infections. Among 50 randomly selected participants in the doxycycline-PEP group, doxycycline was detected in 58 of 200 hair samples (29.0%). All N. gonorrhoeae-positive isolates were resistant to doxycycline. CONCLUSIONS: Among cisgender women, the incidence of STIs was not significantly lower with doxycycline PEP than with standard care. According to hair-sample analysis, the use of doxycycline PEP among those assigned to receive it was low. (Funded by the National Institutes of Health; dPEP ClinicalTrials.gov number, NCT04050540.).
Assuntos
Anti-Infecciosos , Infecções por Chlamydia , Doxiciclina , Gonorreia , Profilaxia Pré-Exposição , Sífilis , Feminino , Humanos , Infecções por Chlamydia/microbiologia , Infecções por Chlamydia/prevenção & controle , Chlamydia trachomatis , Doxiciclina/administração & dosagem , Doxiciclina/efeitos adversos , Doxiciclina/análise , Doxiciclina/uso terapêutico , Infecções por HIV/prevenção & controle , Quênia/epidemiologia , Neisseria gonorrhoeae , Profilaxia Pré-Exposição/métodos , Infecções Sexualmente Transmissíveis/prevenção & controle , Sexo sem Proteção , Anti-Infecciosos/administração & dosagem , Anti-Infecciosos/efeitos adversos , Anti-Infecciosos/análise , Anti-Infecciosos/uso terapêutico , Adolescente , Adulto Jovem , Adulto , Gonorreia/microbiologia , Gonorreia/prevenção & controle , Treponema pallidum , Sífilis/microbiologia , Sífilis/prevenção & controle , Monitoramento de Medicamentos/métodos , Cabelo/químicaRESUMO
Real-time quantitative analysis of tetracyclines is urgently needed to provide consumers with early warning of potential risks. Herein, we report a dual-mode green emissive fluorescent probe, which refers to the liquid mode and the solid mode of electrospun films doped with nitride-doped carbon nanosheets (NCNSs) for real-time detection of doxycycline (DOX). Highly fluorescent NCNSs were prepared by low-temperature solid treatment of urea and sodium citrate. With the addition of DOX, the green emission intensity of NCNSs at 475 nm can be obviously reduced. Method validation exhibited a good linear relationship in 0.05-150 µM between the fluorescence quenching of NCNSs and the concentration of DOX with a limit of detection (LOD) of 0.0127 µM. Furthermore, the immobilization of NCNSs in PAN carriers forming electrospun films stabilizes the green fluorescence of NCNSs. Additionally, electrospun films integrated into a smartphone were developed for real-time detection of DOX with LOD of 0.285 µM. Additionally, DOX in milk was monitored with satisfactory recoveries. Therefore, the integration of the smartphone and electrospun film provides a promising and convenient method for real-time identification of DOX in food analysis.
Assuntos
Doxiciclina , Corantes Fluorescentes , Animais , Doxiciclina/análise , Leite/química , Smartphone , Antibacterianos/análiseRESUMO
The non-scientific disposal of antibiotics has resulted in massive contamination of the bioactive molecules in the aquatic ecosystem. The presence of antibiotics in the effluents limits the biodegradation of micropollutants by affecting the micro-ecological balance. Hence this study aims to remove doxycycline antibiotics from wastewater using biochar. Elemental analysis of the biochar revealed C, Si and N as most abundant content while BET analysis confirmed the mesoporous nature of the adsorbent. The XRD and Raman spectra confirmed amorphic sp2 carbon dominant structure in the biochar. The adsorption mechanism was predicted, correlating the charge distribution and FTIR analysis. The effects of different process parameters were studied using CCD, ANOVA, and RSM. Moreover, the different kinetic models revealed that the pseudo-second-order kinetics model was the best fit and film layer diffusion was the dominant contributor. The isotherm study indicated the high adsorption capacity of the biochar and its non-ionic nature. Thermodynamics study established the spontaneity and exothermic nature. The results suggested no significant change in antibiotic removal efficiency across different system (pond water (97.13%), river water (98.11%), seawater (96.84%), tap water (99.13%), and distilled water (99.74%)). For the desorption of the antibiotic from the biochar surface, 90% ethanol was the most efficient (98.9%), and upon recrystallization by solvent evaporation, 98.7% of the antibiotic of the initial load was recovered. Hence, the implementation of this described process would enable resource recovery along with water treatment, which is not possible with existing approaches. The cost analysis of the whole process revealed that biochar preparation was the bulk expense and the process would be self-sustainable even if the price of the recovered antibiotic would be set at less than half ($41/kg) of the current market price ($94/kg) of the API. Thus, the process endorses a successful circular economy approach toward societal and economic sustainability.
Assuntos
Antibacterianos , Doxiciclina , Eliminação de Resíduos Líquidos , Poluentes Químicos da Água , Adsorção , Antibacterianos/análise , Antibacterianos/química , Carvão Vegetal/química , Doxiciclina/análise , Doxiciclina/química , Ecossistema , Cinética , Oryza/química , Poluentes Químicos da Água/análise , Poluentes Químicos da Água/química , Eliminação de Resíduos Líquidos/métodosRESUMO
Tetracycline pollution in soil irreversibly damages the biosafety of plants by inhibiting the mitochondrial function. Some traditional Chinese medicine (TCM) plants, such as Salvia miltiorrhiza Bunge, have a strong tolerance to mitochondrial damage. We comprehensively compared the doxycycline (DOX) tolerances of two ecotypes of S. miltiorrhiza in the Sichuan and Shandong provinces and found that the Sichuan ecotype had a lower yield reduction, more stable accumulation of medicinal ingredients, higher mitochondrial integrity, and a more robust antioxidant system. The synergetic response networks under DOX pollution of both ecotypes were constructed using RNA sequencing and ultrahigh-performance liquid chromatography-tandem mass spectrometry. The differentiation of the downstream pathways of aromatic amino acids (AAAs) produced variations in the DOX tolerance of S. miltiorrhiza in different regions. The Sichuan ecotype maintained redox homeostasis and xylem development by activating salvianolic acid and indole biosynthesis, while the Shandong ecotype balanced chemical and mechanical defenses by regulating the flavonoid biosynthesis. Rosmarinic acid, a downstream AAA molecule, maintains the mitochondrial homeostasis of plant seedlings under DOX pollution by targeting the ABCG28 transporter. We also highlight the significance of downstream AAA small molecules in guiding the development of bio-based environmental pollution remediation agents.
Assuntos
Salvia miltiorrhiza , Salvia miltiorrhiza/química , Salvia miltiorrhiza/genética , Salvia miltiorrhiza/metabolismo , Doxiciclina/farmacologia , Doxiciclina/análise , Doxiciclina/metabolismo , Ecótipo , Multiômica , Poluição Ambiental , Raízes de Plantas/química , Raízes de Plantas/metabolismoRESUMO
The threat of tetracycline antibiotics to the environment and human health is attracting widespread attention. The development of morphological analysis and quantitative techniques of multiple tetracyclines is of great significance for the evaluation of biochemical toxicity, wide-spectrum antibacterial property and degradation cycle between different tetracyclines. In this study, the white fluorescent Eu/Tb@CDs was synthesized and applied successfully to the identification and detection of the most widely used tetracycline antibiotics (tetracycline (TC), oxytetracycline (OC), chlortetracycline (CC) and doxycycline (DC)) with detection limits all below 1 nM. For the actual water samples with coexistence of the above 4 tetracyclines, their simultaneous morphology identification and accurate quantitative detection can also be realized through simple spectrometric measurement. In addition, the selective and competitive experiments have been carried out on the pollutants widely present in water, and the results have also confirmed that other pollutants could not interfere with the detection of the above 4 tetracyclines. It is undeniable that this work will conveniently and visually reveal the existence information and geographical distribution characteristics of different tetracycline antibiotics in the environment and their action mechanism on organisms.
Assuntos
Clortetraciclina , Oxitetraciclina , Antibacterianos/análise , Doxiciclina/análise , Corantes Fluorescentes/análise , Humanos , Oxitetraciclina/análise , Tetraciclina/análise , Tetraciclinas/análise , ÁguaRESUMO
BACKGROUND: Gingival pigmentation is a discoloration of the gingiva due to a variety of lesions and conditions associated with several endogenous and exogenous etiologic features. OBJECTIVE: The purpose of this study is to describe a report of gingival pigmentation in a patient who used doxycycline. CASE REPORT: A 21-year-old Caucasian female was under dermatological treatment and antibiotic therapy with doxycycline 100 mg (one time a day) for 90 days. She presented brown pigmentation at the gingival margin on the facial surfaces of the upper and lower anterior incisors and premolars. The patient was evaluated by immunohistochemical (S-100, Melan-A, and HMB-45) and histopathologic analyses, and clinical history. Blood levels of malondialdehyde (MDA), glutathione (GSH), and superoxide dismutase (SOD) were analyzed by UV/Vis spectroscopy. The adrenaline, noradrenaline, and dopamine in blood were analyzed by high-performance liquid chromatography (HPLC); dehidroepiandrosterone (DHEA) in serum by radioimmunoassay; and luteinizing hormone (LH) and 25-Hydroxyvitamin D by chemiluminescence. Hematoxylin-eosin stained sections revealed keratinocytes with pigment compatible with melanin. The Fontana-Masson staining was positive in melanophages and in some basal keratinocytes. S-100, Melan A and HMB-45 were confirmed as positive markers of melanocytic differentiation in gingival tissue. We observed a significant increase in malondialdehyde (pË0.05) and a decrease in superoxide dismutase levels (pË0.05). The dopamine value was found to be 15 pg/ml (reference value ≤ 10 pg/ml). CONCLUSION: The use of doxycycline is associated with an increase in oxidative stress and of dopamine with melanin pigments in the gingival tissue. This case report showed a cause-effect relationship between exposure to doxycycline and pigmentation of the marginal gingiva.
Assuntos
Doxiciclina , Gengiva , Humanos , Feminino , Adulto Jovem , Adulto , Gengiva/química , Doxiciclina/efeitos adversos , Doxiciclina/análise , Melaninas/análise , Dopamina/análise , Superóxido Dismutase/análise , Malondialdeído/análiseRESUMO
Manure is a major source of soil and plant contamination with veterinary drugs residues. The aim of this study was to evaluate the uptake of 14 veterinary pharmaceuticals by parsley from soil fertilized with manure. Pharmaceutical content was determined in roots and leaves. Liquid chromatography coupled with tandem mass spectrometry was used for targeted analysis. Screening analysis was performed to identify transformation products in the parsley tissues. A solid-liquid extraction procedure was developed combined with solid-phase extraction, providing recoveries of 61.9-97.1% for leaves and 51.7-95.6% for roots. Four analytes were detected in parsley: enrofloxacin, tylosin, sulfamethoxazole, and doxycycline. Enrofloxacin was detected at the highest concentrations (13.4-26.3 ng g-1). Doxycycline accumulated mainly in the roots, tylosin in the leaves, and sulfamethoxazole was found in both tissues. 14 transformation products were identified and their distribution were determined. This study provides important data on the uptake and transformation of pharmaceuticals in plant tissues.
Assuntos
Poluentes Ambientais , Poluentes do Solo , Drogas Veterinárias , Doxiciclina/análise , Enrofloxacina/análise , Poluentes Ambientais/análise , Esterco/análise , Petroselinum , Solo/química , Poluentes do Solo/análise , Extração em Fase Sólida/métodos , Sulfametoxazol , Tilosina , Drogas Veterinárias/análiseRESUMO
OBJECTIVE: To understand the monitoring status of veterinary drug residues in chickens and eggs sold in Ningxia from 2016 to 2020, and to evaluate the health risks of human intake. METHODS: A total of 303 chicken and 237 eggs were collected from 2016 to 2020, and the veterinary drug residues in chickens and eggs sold in Ningxia were detected and analyzed by high performance liquid chromatography-tandem mass spectrometry. The food safety index method was used to assess the health risks in combination with the dietary intake of residents. RESULTS: The detection rate of veterinary drug residues in chicken was 38.0%(115/303), and the over-standard rate was 7.6%(23/303). The detection rate of veterinary drug residues in eggs was 26.6%(63/237), and the over-standard rate was 19.8%(47/237). The food safety index of doxycycline in chicken was 4.59, and the food safety indexes of doxycycline, flumequine and flufenicol in eggs were 7.09, 26.5 and 2.33, respectively, all of which were much higher than 1, suggesting that there were health risks. The food safety indexes of other substances were all less than 1, and the food safety indexes were all acceptable. CONCLUSION: Veterinary drugs were widely detected in chicken and eggs in Ningxia from 2016 to 2020. Some veterinary drugs had hidden health risks.
Assuntos
Resíduos de Drogas , Drogas Veterinárias , Cromatografia Líquida de Alta Pressão/métodos , Doxiciclina/análise , Resíduos de Drogas/análise , Ovos/análise , Contaminação de Alimentos/análise , Medição de Risco , Espectrometria de Massas em Tandem/métodos , Drogas Veterinárias/análiseRESUMO
The overuse of antibiotics in recent years presents a huge challenge to society for their removal from the environment. The prolonged presence of antibiotics as environmental pollutants results in the emergence of drug-resistant bacteria faster than new antibiotics to treat diseases they cause. Therefore, a rapid, sensitive, and cost-effective method is urgently required to detect and degrade antibiotics. Given this, a novel strategy has been devised for synthesizing Fe-doped carbon dots (Fe-N@CDs) and iron oxide-carbon dot hybrid nanoparticles (Fe3O4-CDs) in a single step for doxycycline detection and its degradation. For the very first time, the formation of two simultaneous products, i.e., Fe-N@CDs (0 D fluorescent carbon dots) and Fe3O4-CDs (magnetic nanoparticles) in a single step hydrothermal carbonization process by using a sole iron salt (FeCl2) and carbon precursor (citric acid) in the presence of ethylenediamine is reported. The as prepared Fe-N@CDs selectively detect doxycycline with a limit of detection value of 66 ng mL-1 and in the linear range from 0 mg mL-1 to 50 mg mL-1, whereas the other formed products, i.e., Fe3O4-CDs, degrade doxycycline by 70.26% in just 5 min by applying shear force using simply a kitchen blender. The results demonstrated the suitability and application scope in food and environment safety.
Assuntos
Doxiciclina/análise , Recuperação e Remediação Ambiental/métodos , Nanopartículas , Pontos Quânticos , Poluentes da Água/análise , Antibacterianos/análise , Antibacterianos/metabolismo , Carbono , Doxiciclina/metabolismo , Monitoramento Ambiental/métodos , ÁguaRESUMO
Doxycycline residues in claws may pose a potential risk to humans. A study with broiler chickens was performed to find the concentrations of doxycycline in claws after treatment. For the quantification of the antibiotic of interest in claws, an ultrahigh-performance liquid chromatography-tandem mass spectrometry method was developed. Doxycycline was detectable at 3043 µg/kg at sub-therapeutic treatment, 223 µg/kg after therapeutic doses, and 14 µg/kg after spray application on the last day of the experiment (day 22). Almost 70 days is required for the concentration of doxycycline to reach zero. The obtained results show that monitoring of doxycycline in claws should be implemented.
Assuntos
Resíduos de Drogas , Casco e Garras , Animais , Antibacterianos/análise , Galinhas , Cromatografia Líquida de Alta Pressão/métodos , Doxiciclina/análise , Resíduos de Drogas/análise , Casco e Garras/química , Humanos , Saúde Pública , Espectrometria de Massas em Tandem/métodosRESUMO
The residue problem of tetracycline antibiotics, especially doxycycline (DC), in animal foodstuffs has attracted much attention. This paper reported ZIF-8 and bovine serum albumin (BSA) as a ratiometric fluorescence-scattering sensor for DC. The mechanism relied on the disassembly of ZIF-8 caused by DC, bringing weakened second-order scattering, and the double fluorescence amplification of DC under ZIF-8 with BSA, inducing enhanced fluorescence. The response of the sensor was completed within 1 min, and the detection limit for DC (3.4 nM) was 1-2 orders of magnitude lower than the reported ones. The distinguishment of DC from other tetracycline antibiotics was also achieved by the sensor. The sensor was applied to detecting DC in animal foodstuffs with satisfactory recoveries (80.0-104.0%). Hence, this work develops a rapid, sensitive and selective ratiometric sensor to monitor the DC residue in animal foodstuffs, also opens the window to construct ratiometric DC sensors with the fluorescence-scattering strategy.
Assuntos
Doxiciclina , Contaminação de Alimentos/análise , Carne/análise , Pontos Quânticos , Animais , Antibacterianos , Doxiciclina/análise , Corantes Fluorescentes , Limite de Detecção , Soroalbumina Bovina , Espectrometria de FluorescênciaRESUMO
An innovative, rapid and stable method for simultaneous determination of three tetracycline (oxytetracycline, tetracycline and doxycycline) and two fluoroquinolone (ciprofloxacin and enrofloxacin) residues in poultry eggs by ultra-high performance liquid chromatography-fluorescence detection (UPLC-FLD) was established and optimized. The samples were homogenized and extracted with acetonitrile/ultrapure water (90:10, v/v) and then purified by solid-phase extraction (SPE). LC separation was achieved on an ACQUITY UPLC BEH C18 column (1.7 µm, 2.1 mm × 100 mm), and the mobile phase was composed of acetonitrile and a 0.1 mol/L malonic acid solution containing 50 mmol/L magnesium chloride (the pH was adjusted to 5.5 with ammonia). When the five target drugs were spiked at the limit of quantification, 0.5 times the maximum residue limit (MRL), 1.0 MRL and 2.0 MRL, the recoveries were above 83.5% and the precision ranged from 1.99% to 6.24%. These figures of merit complied with the parameter validation regulations of the EU and U.S. FDA. The limits of detection and quantifications of the targets were 0.1-13.4 µg/kg and 0.3-40.1 µg/kg, respectively. The proposed method was easily extended to quantitative analyses of target drug residues in 85 egg samples, thus demonstrating its reliability and applicability.
Assuntos
Antibacterianos/análise , Cromatografia Líquida de Alta Pressão/métodos , Ovos/análise , Fluoroquinolonas/análise , Espectrometria de Fluorescência/métodos , Tetraciclinas/análise , Animais , Ciprofloxacina/análise , Doxiciclina/análise , Resíduos de Drogas/análise , Enrofloxacina/análise , Contaminação de Alimentos/análise , Limite de Detecção , Oxitetraciclina/análise , Aves Domésticas , Reprodutibilidade dos Testes , Extração em Fase Sólida , Tetraciclina/análise , Drogas Veterinárias/análiseRESUMO
The residue of doxycycline in food can cause harm to human. Therefore, the detection of doxycycline residue is necessary. Herein, a ratiometric fluorescent probe was designed based on sulfur quantum dots (S dots) and Ca2+. Due to static quenching and inter filter effect between doxycycline and S dots, doxycycline quenched fluorescence of S dots at 450 nm. Meanwhile, doxycycline and Ca2+ formed fluorescent complex through coordination to produce new peak at 520 nm. The ratio of fluorescence intensity (F520/F450) and doxycycline concentration showed good linear relationship with detection limit of 0.19 µM. The fluorescence color of S dots/Ca2+ changed from blue to light green with increasing doxycycline concentration, which was applied for visual semi-quantitative detection of doxycycline. Moreover, the method was used for detecting doxycycline in milk and fish samples with recoveries in the range of 91%-110%. The method showed good application potential in detection of doxycycline in food samples.
Assuntos
Cálcio/química , Doxiciclina/análise , Corantes Fluorescentes/química , Análise de Alimentos/métodos , Limite de Detecção , Pontos Quânticos/química , Enxofre/química , Animais , Doxiciclina/química , Contaminação de Alimentos/análise , Humanos , Leite/química , Espectrometria de FluorescênciaRESUMO
Residues of veterinary drugs in poultry meat have serious health effects on humans (e.g., antimicrobial resistance, carcinogenicity, and hypersensitivity), which make the control of veterinary drug residues an important parameter in ensuring consumer protection. This work was performed to quantitatively determine two co-formulated anti-infective veterinary agents, tylosin tartrate (TYT) and doxycycline hydrochloride (DOX) in different tissues of broiler chickens (liver, muscles, and fat) using high performance liquid chromatography. The chicken was treated with the recommended dose of a binary mixture of the drugs (Tydovet). Moreover, the study aimed to estimate the withdrawal time of both drugs in chicken tissues. The analysis was done by solvent extraction and solid-phase extraction for clean-up of samples from the tissue matrix, followed by liquid chromatographic determination of the cited drugs with UV-detection. Residue decline with time was tracked, and both antibiotics were found to be more persistent in liver tissues than other tissues (muscle and fat). The effect of freezing and cooking was investigated on tissue residue levels. While freezing had little effect on the concentration of both antibiotics; cooking, as anticipated, led to a marked decline. Therefore, it is recommended to pay attention to the proper withdrawal periods before marketing to ensure the hygienic suitability of broilers edibles for safe human consumption. PRACTICAL APPLICATION: This novel study measures tylosin and doxycycline residues simultaneously in different tissues (muscle, fat, and liver) after administration of Tydovet powder to the broiler chicken. Residues in fat persisted for a longer time than in muscle in case of TYT, whereas the reverse was noticed in DOX.
Assuntos
Antibacterianos/análise , Doxiciclina/análise , Resíduos de Drogas/análise , Carne/análise , Tilosina/análise , Drogas Veterinárias/análise , Animais , Galinhas , Análise de Alimentos , Humanos , Fígado/metabolismo , Músculos/metabolismo , Fatores de TempoRESUMO
In clinical chemistry, frequent monitoring of drug levels in patients has gained considerable importance because of the benefits of drug monitoring on human health, such as the avoidance of high risk of over dosage or increased therapeutic efficacy. In this work, we demonstrate that the drug doxycycline can act as an Au nanoparticle (doxy-AuNP) growth and capping agent to enhance the response of a surface plasmon resonance (SPR) biosensor for this drug. SPR analysis revealed the high sensitivity of doxy-AuNPs towards the detection of free doxycycline. More specifically, doxy-AuNPs bound with protease-activated receptor-1 (PAR-1) immobilized on the SPR sensing surface yield the response in SPR, which was enhanced following the addition of free doxy (analyte) to the solution of doxy-AuNPs. This biosensor allowed for doxycycline detection at concentrations as low as 7 pM. The study also examined the role of colloidal stability and growth of doxy-AuNPs in relation to the response-enhancement strategy based on doxy-AuNPs. Thus, the doxy-AuNPs-based SPR biosensor is an excellent platform for the detection of doxycycline and demonstrates a new biosensing scheme where the analyte can provide enhancement.