BiOBr/FeMoO4 composite achieves oxygen vacancy concentration adjustment to promote persulfate activation degradation of organic pollutants in saline water.

The investigation about the mechanism of crystal plane regulation on the generation of oxygen vacancies remains a challenge. In this paper, BiOBr/FeMoO4 composites were synthesized by precise control of crystal plane growth, and it exhibited the enhanced concentration of oxygen vacancies due to lower formation energy of oxygen vacancies. The composite performs higher photo-Fenton-like ability for degrading oxytetracycline hydrochloride (OTC). Structural analyses and theoretical calculations reveal that crystal plane regulation induces significant changes in oxygen vacancy concentration. The BiOBr/FeMoO4/peroxydisulphate (PDS) /light system, which dominated by the non-radical pathway, degraded 96.8 % ± 1.0 % of OTC within 30 min. The activation mechanism of the system and the degradation pathway of OTC were elucidated. The intermediates in the degradation process of OTC were evaluated using liquid chromatograph-mass spectrometer (LC-MS), toxicity evaluation software tool (T.E.S.T) and soybean germination experiments. This work offers novel insights into the pivotal role of crystal plane directional regulation in the quantitative generation of oxygen vacancies.

Adsorptive removal of oxytetracycline hydrochloride using bagasse-based biochar powder and beads.

Oxytetracycline Hydrochloride (OTC), a common antibiotic used to treat specific illnesses in humans and animals, is characterized by poor absorption into cells, low volatility, and high hydrophilicity. It is a potent contaminant that poses a serious threat to the ecosystem, particularly the aquatic sources. Adsorption onto natural adsorbents is one of the most successful, economical, and ecologically friendly ways to remove antibiotics from waste water. The present work focuses on the adsorption of OTC utilizing alginate biochar beads (AlBCB) and biochar powder (BC) derived from bagasse. The influence of several factors were studies and optimized through batch studies employing BC and AlBCB. After 50 min BC displayed a removal of 97%, at an initial concentration of 10 ppm. The experimental data was discovered to follow PFO kinetics and fit with the Freundlich isotherm adsorption model. AlBCB, after a contact time of 40 min, indicated a maximum percentage removal of 86% for initial concentration of 10 ppm OTC. Al-biochar beads showed the maximum percentage removal at pH 10. 0.5 g of adsorbent was used to carry out all batch experiments at room temperature. The adsorption fitted Freundlich adsorption isotherm and intraparticle diffusion kinetics.

[Adsorption Performance and Mechanism of Oxytetracycline in Water by KOH Modified Biochar Derived from Corn Straw].

The pollution control of tetracycline antibiotics in the environment has become a hot topic, and biochar adsorption has become an important technology to remove organic pollutants. Pyrolytic biochars (BC400, BC500, and BC600) were prepared from corn straw and then were modified by KOH to obtain KBC400, KBC500, and KBC600. Among them, KBC400 was selected for secondary pyrolysis activation at 400-600℃ to obtain AKBC400, AKBC500, and AKBC600. The structure characteristics and surface properties of AKBC were also characterized. The adsorption kinetics and thermodynamic characteristics of oxytetracycline hydrochloride (OTC) in the solution by AKBC were investigated using batch experiments. Compared to that of BC400, the specific surface area and pore structure of AKBC were significantly improved, and the aromaticity was also enhanced, resulting in the notable enhancement of the adsorption capacities for OTC. The pseudo-second-order kinetics model could better fit the adsorption process, and AKBC500 had the largest adsorption rate constant and capacity. Both the intraparticle diffusion and film diffusion were the rate-limiting steps. The Langmuir, Freundlich, and Temkin models could fit the adsorption isotherms perfectly. The adsorption of OTC on AKBC was a spontaneous, endothermic, and entropy-increasing process by both physisorption and chemisorption. The pH values in the range of 3.0-7.0 were favorable for the adsorption of OTC by AKBC. The adsorption capacity decreased with the humic acid concentration over 10 mg·L-1. The adsorption mechanism of OTC by AKBC involved pore filling, hydrogen bonding, π-π conjugation, cation-π bond, and strong electrostatic effect. AKBC still had good reusability for OTC removal after five times of regeneration. The obtained AKBC is a potential adsorbent for OTC removal from water due to the good pore structure, high adsorption capacity, and stable adsorption effect.

Influences of Jujube Witches' Broom (JWB) Phytoplasma Infection and Oxytetracycline Hydrochloride Treatment on the Gene Expression Profiling in Jujube.

Jujube witches' broom disease (JWB), caused by Candidatus Phytoplasma ziziphi, is the most destructive phytoplasma disease threatening the jujube industry. Tetracycline derivatives treatments have been validated to be capable of recovering jujube trees from phytoplasma infection. In this study, we reported that oxytetracycline hydrochloride (OTC-HCl) trunk injection treatment could recover more than 86% of mild JWB-diseased trees. In order to explore the underlying molecular mechanism, comparative transcriptomic analysis of healthy control (C group), JWB-diseased (D group) and OTC-HCl treated JWB-diseased (T group) jujube leaves was performed. In total, 755 differentially expressed genes (DEGs), including 488 in 'C vs. D', 345 in 'D vs. T' and 94 in 'C vs. T', were identified. Gene enrichment analysis revealed that these DEGs were mainly involved in DNA and RNA metabolisms, signaling, photosynthesis, plant hormone metabolism and transduction, primary and secondary metabolisms, their transportations, etc. Notably, most of the DEGs identified in 'C vs. D' displayed adverse change patterns in 'D vs. T', suggesting that the expression of these genes was restored after OTC-HCl treatment. Our study revealed the influences of JWB phytoplasma infection and OTC-HCl treatment on gene expression profiling in jujube and would be helpful for understanding the chemotherapy effects of OTC-HCl on JWB-diseased jujube.

Degradation of oxytetracycline by iron-manganese modified industrial lignin-based biochar activated peroxy-disulfate: Pathway and mechanistic analysis.

In this study, high-performance Fe-Mn-modified industrial lignin-based biochar (FMBC) was successfully prepared to facilitate the efficient degradation of oxytetracycline by its driven sulfate radical-based advanced oxidation process with 90% degradation within 30 min. The results showed that oxygenated functional groups (e. g. hydroxyl, carbonyl, etc.) in industrial lignin-based biochar, the synergistic effect of transition metals Fe and Mn, and defective structures were the active sites for activation of peroxy-disulfate. SO4·- produced during the degradation process assumed a key function. Significantly, 38 intermediates were innovatively proposed for the first time in the system, and oxytetracycline was degraded in 7 ways, including deamidation, demethylation, hydroxylation, secondary alcohol oxidation, ring opening, dehydration, and carbonylation. A new perspective on the application of industrial lignin in the advanced oxidative degradation of organic pollutants was provided by this study.

Preparation of Biochar with Developed Mesoporous Structure from Poplar Leaf Activated by KHCO3 and Its Efficient Adsorption of Oxytetracycline Hydrochloride.

The effective removal of oxytetracycline hydrochloride (OTC) from the water environment is of great importance. Adsorption as a simple, stable, and cost-effective technology is regarded as an important method for removing OTC. Herein, a low-cost biochar with a developed mesoporous structure was synthesized via pyrolysis of poplar leaf with potassium bicarbonate (KHCO3) as the activator. KHCO3 can endow biochar with abundant mesopores, but excessive KHCO3 cannot continuously promote the formation of mesoporous structures. In comparison with all of the prepared biochars, PKC-4 (biochar with a poplar leaf to KHCO3 mass ratio of 5:4) shows the highest adsorption performance for OTC as it has the largest surface area and richest mesoporous structure. The pseudo-second-order kinetic model and the Freundlich equilibrium model are more consistent with the experimental data, which implies that the adsorption process is multi-mechanism and multi-layered. In addition, the maximum adsorption capacities of biochar are slightly affected by pH changes, different metal ions, and different water matrices. Moreover, the biochar can be regenerated by pyrolysis, and its adsorption capacity only decreases by approximately 6% after four cycles. The adsorption of biochar for OTC is mainly controlled by pore filling, though electrostatic interactions, hydrogen bonding, and π-π interaction are also involved. This study realizes biomass waste recycling and highlights the potential of poplar leaf-based biochar for the adsorption of antibiotics.

Carbon nanotube-loaded copper-nickel ferrite activated persulfate system for adsorption and degradation of oxytetracycline hydrochloride.

In this study, a new composite (MWCNTs-CuNiFe2O4) prepared by loading magnetic CuNiFe2O4 particles onto carboxylated carbon nanotubes (MWCNTs) through co-precipitation was applied to remove oxytetracycline hydrochloride (OTC-HCl) in solution. The magnetic properties of this composite could address of the issue of difficulty associated with the separation of MWCNTs from mixtures when applied as an adsorbent. In addition to the good adsorption properties recorded for MWCNTs-CuNiFe2O4 towards OTC-HCl, this developed composite could be used to activate potassium persulfate (KPS) for an efficient degradation of OTC-HCl. The MWCNTs-CuNiFe2O4 was systematically characterized using Vibrating Sample Magnetometer (VSM), Electron Paramagnetic Resonance (EPR) and X-ray Photoelectron Spectroscopy (XPS). The influence of dose of MWCNTs-CuNiFe2O4, the initial pH, the amount of KPS and the reaction temperature on the adsorption and degradation of OTC-HCl by MWCNTs-CuNiFe2O4 were discussed. The adsorption and degradation experiments showed that MWCNTs-CuNiFe2O4 exhibited an adsorption capacity of 270 mg·g-1 for OTC-HCl with the removal efficiency 88.6% at 303 K (at an initial pH 3.52, 5 mg KPS, 10 mg composite, 10 mL reaction concentration 300 mg·L-1 of OTC-HCl). The Langmuir and Koble-Corrigan models were used to describe the equilibrium process while the Elovich equation and Double constant model were suitable to describe the kinetic process. The adsorption process was based on single-molecule layer reaction and non-homogeneous diffusion process. The mechanisms of adsorption were complexation and hydrogen bond whereas active species such as SO4‧-, ‧OH and 1O2 were confirmed to have played a major role in the degradation of OTC-HCl. The composite was also found to be very stable with good reusability property. These results confirm the good potential associated with the use of MWCNTs-CuNiFe2O4/KPS system for the removal of some typical pollutants from wastewater.

Pharmaceutical Systems as a Strategy to Enhance the Stability of Oxytetracycline Hydrochloride Polymorphs in Solution.

In order to improve the stability of oxytetracycline hydrochloride, a polymorphic antibiotic set of novel binary systems were developed using ß-cyclodextrin and amino acids with different acid-basic characteristics as ligands. The formation constants for each system containing ß-cyclodextrin, L-aspartic acid, histidine and N-acetylcysteine were determined by Scott's method and statistical studies. The structure of the binary systems with ß-cyclodextrin and N-acetylcysteine was elucidated by NMR experiments. The effect ß-cyclodextrin and N-acetylcysteine on the polymorph's chemical stability in aqueous and phosphate buffered saline solutions at 25 °C was monitored by an optimized and validated high-performance liquid chromatography method. The combination of N-acetylcysteine with the three polymorphs and the ß-cyclodextrin system obtained with the form III demonstrated a reduction in the degradation rate of oxytetracycline hydrochloride in the aqueous solution when compared to each free form, with an increase of 20 h in the half time. It evidences that the use of amino acids as ligands constitutes an interesting alternative for pharmaceutical areas. In conclusion, based on the results obtained, these pharmaceutical systems could be candidates for the development of a pharmaceutical formulation for the administration of the drug through reconstituted solutions using the binary system as a promising tool for improving the stability of oxytetracycline hydrochloride polymorphs in solution.

High-capacity removal of oxytetracycline hydrochloride from wastewater via Mikania micrantha Kunth-derived biochar modified by Zn/Fe-layered double hydroxide.

Antibiotic contamination in water has been an increasing global concern, and how to effectively remove antibiotics (e.g., oxytetracycline [OTC] hydrochloride) from wastewater becomes imperative. In this study, the biochar derived from an invasive plant (Mikania micrantha Kunth) was synthesized with Zn/Fe- layered double hydroxide (LDH) by co-precipitation method (ZnFe-LDH/MBC) to remove OTC from water. ZnFe-LDH/MBC posed the highest OTC removal performance of 426.61 mg/g. ZnFe-LDH/MBC exhibited stability and efficiency in OTC adsorption at different pH levels and under interfering conditions with co-existing ions, as well as outstanding regeneration capabilities during adsorption-desorption cycles. Furthermore, the removal of OTC by ZnFe-LDH/MBC was mediated by several processes including pore filling, hydrogen bonding force, electrostatic interaction, π-π interaction, as well as complexation. Consequently, ZnFe-LDH/MBC has excellent potential for the purification of OTC pollutants that is low-cost, efficient, and environmentally friendly.

Performance and mechanism of sycamore flock based biochar in removing oxytetracycline hydrochloride.

In this study, sycamore flocs (SF), which caused environmental and health problems, were utilized to prepare biochar. SFB2-900 obtained under the conditions of activation agent K2CO3, pyrolysis temperature 900℃ and m(K2CO3):m(BC) 2 had the strongest adsorption capacity (730 mg/g) for oxytetracycline hydrochloride (OTC-HCl). The pseudo-second-order kinetic model and Langmuir model described the adsorption kinetics and isotherms best. SFB2-900 exhibited high OTC-HCl adsorption capacity in both higher ionic strength and wide pH range. The theoretical simulation indicated that the closest interaction distance between OTC-HCl and SFB2-900 was 2.44 Å via π-π stacking configuration. Pore filling, π-π electron donor acceptor (EDA) interaction, H-bonding and electrostatic interactions were also involved in the process of OTC-HCl removal. SFB2-900 showed great removal efficiency for OTC-HCl in different water matrices and good regeneration ability. This study solved the problems caused by SF, realized waste biomass recycling, and achieved preparing high-efficient adsorbent for antibiotic.

Community-level and function response of photoautotrophic periphyton exposed to oxytetracycline hydrochloride.

Periphyton is considered important for removal of organic pollutants from water bodies, but knowledge of the impacts of antibiotics on the community structure and ecological function of waterbodies remains limited. In this study, the effects of oxytetracycline hydrochloride (OTC) on the communities of photoautotrophic epilithon and epipelon and its effect on nitrogen and phosphorus concentrations in the water column were studied in a 12-day mesocosm experiment. The dynamics of nitrogen and phosphorus concentrations in the epipelon and epilithon experiment showed similar patterns. The concentrations of total nitrogen, dissolved total nitrogen, ammonium nitrogen, total phosphorus and dissolved total phosphorus in the water column increased rapidly during the initial days of exposure, after which a downward trend occurred. In the epilithon experiment, we found that the photosynthesis (Fv/Fm) and biomass of epilithon were significantly (P < 0.05) stimulated in the low concentration group. Contrarily, growth and photosynthesis (Fv/Fm) were significantly (P < 0.05) reduced in the medium and high concentration group. We further found that the photosynthetic efficiency of photoautotrophic epilithon was negatively correlated with the concentrations of nitrogen and phosphorus in the water column (P < 0.05). Principal coordinate analysis (PCoA) showed that the communities of epilithic algae in the control group and in the low concentration group were significantly (P < 0.05) different from that of the high concentration group during the initial 4 days. After 8 days' exposure, all groups tended to be similar, indicating that epilithon showed rapid adaptability and/or resilience. Similar results were found for the relative abundance of some epilithic algae. Our findings indicate that the biofilm system has strong tolerance and adaptability to OTC as it recovered fast after an initial suppression, thus showing the important role of periphyton in maintaining the dynamic balance of nutrients with other processes in aquatic ecosystems.

Simultaneous analysis of oxytetracycline hydrochloride, lidocaine, and bromhexine hydrochloride in the presence of many interfering excipients.

A gradient elution high-performance liquid chromatographic method with a diode array detector is introduced for the first time for the simultaneous estimation of three drugs, namely, oxytetracycline hydrochloride (OXT), lidocaine (LDC), and bromhexine hydrochloride (BRH), in a veterinary formulation (OxyClear® solution) that contains many interfering additives. The method used a C-8 column. The chromatographic eluting solution included acidified water (0.1% trifluoroacetic acid in water) and acetonitrile at a 1-ml/min flow rate and 254 nm as a nominated detection wavelength. The chromatographic process was assessed in terms of linearity, precision, accuracy, LOD, and LOQ. OXT, LDC, and BRH were linear in the range of 1-60, 5-100, and 1-60 µg/ml, respectively. The three drugs were determined successfully without the interference of three excipients having UV absorbances. Furthermore, the purities of the peaks of the three drugs were confirmed by comparing the UV spectra of investigated peaks to the UV reference spectra in Clarke's Analysis of Drugs and Poisons. The greenness value of the method was 0.69 with a faint green-colored pictogram using the AGREE tool. These merits recommend the application of the planned method in QC laboratories for purity testing and concentration assays for the pure drugs and commercial formulations.

Effect of Oxytetracycline-Hydrochloride on Phytoplasma Titer and Symptom Progression of the 16SrIV-D Phytoplasma in Cabbage Palms from Florida.

Lethal bronzing (LB) is a phytoplasma disease of palms in Florida, U.S.A. Historically, the use of the antibiotic oxytetracycline-hydrochloride (OTC-HCl) was optimized to treat for LY, and currently label rates for OTC-HCl developed for LY are being used to treat palms preventatively against LB. Because of the economic impact of LB, assessing OTC-HCl against LB is essential for developing and optimizing management options for this disease. In this study, Sabal palmetto palms declining from LB were injected with OTC-HCl to assess efficacy on LB. Four groups of palms were selected that represented healthy palms, early symptomatic palms, palms with moderate symptoms, and palms with late-stage symptoms. Within each group, treatment palms injected with OTC-HCl and a control group with no antibiotics were tested weekly by quantitative PCR for 1 year. For asymptomatic palms, treated palms never developed symptoms or tested positive, whereas one of the control palms did. The early symptomatic palms that were treated had similar levels of phytoplasma to the control group but had much slower symptom development. Palms with moderate symptoms had no difference in titer between the treatment and the control group, but treated palms had much slower symptom development. Palms with late-stage symptoms showed no difference in phytoplasma titer or symptom progression between treated and control palms. These results suggest that label rates of OTC-HCl appear useful as a preventative against LB, but once symptoms develop, label rates cannot cure palms. In the meantime, removal of symptomatic palms is recommended.

Exploring solid forms of oxytetracycline hydrochloride.

Oxytetracycline hydrochloride, an antibiotic of the tetracycline family, is a polymorphic drug that evidences erratic absorption in oral administration. Additionally, poor solid state characterization of the polymorphs and diversity in the existing nomenclature impede the correct identification of the raw materials. In this work, oxytetracycline hydrochloride solid forms were prepared from isopropyl alcohol, ethanol and methanol through different crystallization techniques, and then their physicochemical and microbiological properties were evaluated. A combination of advanced techniques such as solid state nuclear magnetic resonance, powder X-ray diffraction, infrared spectroscopy, thermal analysis, scanning electron microscopy and energy-dispersive X-ray spectroscopy were used in the characterization of solid samples giving clear evidence of the existence of three stable and one metastable solid forms of the oxytetracycline hydrochloride. Solubility was determined in aqueous solution, simulated gastric fluid, and simulated intestinal fluid. In addition, microbiological studies were performed. The polymorphs showed similar antimicrobial activity against Escherichia coli and Staphylococcus aureus. Therefore, these solid forms of oxytetracycline hydrochloride constitute promising candidates to encourage studies for repositioning old and known antibiotic drugs in the developing strategies for new therapeutic alternatives.

UV/Vis Light Induced Degradation of Oxytetracycline Hydrochloride Mediated byCo-TiO2 Nanoparticles.

Pharmaceuticals, especially antibiotics, constitute an important group of aquatic contaminants given their environmental impact. Specifically, tetracycline antibiotics (TCs) are produced in great amounts for the treatment of bacterial infections in both human and veterinary medicine. Several studies have shown that, among all antibiotics, oxytetracycline hydrochloride (OTC HCl) is one of the most frequently detected TCs in soil and surface water. The results of the photocatalytic degradation of OTC HCL in aqueous suspensions (30 mg·L-1) of 0.5 wt.% cobalt-doped TiO2 catalysts are reported in this study. The heterogeneous Co-TiO2 photocatalysts were synthesized by two different solvothermal methods. Evonik Degussa Aevoxide P25 and self-prepared TiO2 modified by the same methods were used for comparison. The synthesized photocatalysts were characterized by X-ray powder diffraction (XRD), Raman spectroscopy, transmission electron microscopy (TEM), UV/vis diffuse reflectance spectroscopy (DRS), and N2 adsorption (BET) for specific surface area determination. The XRD and Raman results suggest that Ti4+ was substituted by Co2+ in the TiO2 crystal structure. Uv/visible spectroscopy of Co-TiO2-R showed a substantial redshift in comparison with bare TiO2-R. The photocatalytic performance of the prepared photocatalysts in OTC HCL degradation was investigated employing Uv/vis spectroscopy and high-performance liquid chromatography (HPLC). The observed initial reaction rate over Co-TiO2-R was higher compared with that of Co-TiO2-HT, self-prepared TiO2, and the commercial P25. The enhanced photocatalytic activity was attributed to the high surface area (153 m2·g-1) along with the impurity levels within the band gap (2.93 eV), promoting the charge separation and improving the charge transfer ability. From these experimental results, it can be concluded that Co-doping under reflux demonstrates better photocatalytic performances than with the hydrothermal treatment.

Polycaprolactone nanofibers loaded oxytetracycline hydrochloride and zinc oxide for treatment of periodontal disease.

Periodontal diseases (PD) are mixed bacterial infections caused by microorganisms that colonize the tooth surface, leading to destructions at tooth-supporting tissues. Several local delivery systems, as nanofibers, have been developed for the treatment of PD. The purpose of the present study was developing polycaprolactone (PCL) nanofibers incorporating two antibacterial agents, OTC and ZnO, for use in the treatment of PD. Nanofibers were produced by electrospinning method: PCL loaded with ZnO (PCL-Z), PCL loaded with OTC (PCL-OTC), PCL loaded with OTC and ZnO (PCL-OTCz) and pristine PCL (PCL-P). The nanofibers were characterized physicochemically using different techniques. In addition, in vitro study of the OTC release from the nanofibers was performed. The PCL-OCT showed sustained release of the drug up to 10 h, releasing 100% of OTC. However, the PCL-OTCz nanofiber showed a slow release of OTC up to 120 h (5th day) with 54% of drug retention. The cytotoxicity assay showed that PCL-OTC nanofiber was slightly cytotoxic after 48 h and the other nanofibers were non-cytotoxic. The antibacterial activity of the nanofibers was evaluated by qualitative and quantitative analysis and against mixed bacterial culture, composed of four Gram-negative anaerobic bacteria involved in periodontal diseases. The disk diffusion method showed that the PCL-OTC displayed higher inhibition zone than PCL-OTCz (p < 0.001). The quantitative analysis, evaluated by broth culture, showed that the PCL-OTC and PCL-OTCz exhibited excellent activity against a mixed bacterial culture with growth inhibition of 98.0% and 97.5%, respectively. Based on these results, the PCL-OTCz nanofibers developed have great potential as a drug delivery system for the PD treatment.

Determination of oxytetracycline hydrochloride in milk and egg white samples using Ru(bipy)3 2+ -Ce(SO4 )2 chemiluminescence.

A novel, rapid and sensitive chemiluminescence (CL) method for the determination of oxytetracycline hydrochloride (OTCH) is described in this paper. The presented method was based on the fact that OTCH could immensely enhance the CL of the reaction of cerium sulfate and tris(2,2-bipyridyl) ruthenium (II) in acidic medium. Under optimal experimental conditions, CL intensity was favorably linear for OTCH in the range 5.0 × 10-7 to 5.0 × 10-5  g/ml, with a detection limit of 1.5 × 10-7  g/ml (S/N = 3). The relative standard detection was 4.76% for 5.0 × 10-6  g/ml (n = 11). This method was successfully applied to the analysis of OTCH in milk and egg white samples. According to the results of the kinetic curves for OTCH in the Ru(bipy)3 2+ -Ce(SO4 )2 CL system, together with CL and ultraviolet (UV)-visible spectra, the possible mechanism of the CL reaction is discussed briefly.

Validation of daily microincrement deposition in otoliths of juvenile and adult Peruvian anchovy Engraulis ringens.

Wild adult specimens of the Peruvian anchovy Engraulis ringens were captured and reared to validate the daily periodicity of otolith microincrement formation. The postcapture stress generated spontaneous spawning, making it possible to conduct a rearing trial on larvae first in an artificial nutrient-enriched system (ANES) for 52 days followed by an artificial feeding regime in a culture tank until day 115 post-hatch. Microincrements of the sagittal otoliths of sacrificed juveniles [mean ± S.D. total length (LT ) = 5·13 ± 0·37 cm, range 5-6 cm; c.v. = 7·5%] showed very distinct light and dark zones. The slope of the relationship between the total number of increments after the hatch check and days elapsed after hatching was not significantly different from 1. The transfer from ANES to the artificial feeding regime induced a mark in the sagittal otoliths. The number of microincrements after this induced mark coincided with the number of days elapsed after the transfer date. In parallel experiments, adult E. ringens (mean ± S.D. LT = 14·92 ± 0·55 cm, range 13-16 cm) were exposed to one of two fluorescent marking immersion treatments with either alizarin red S (ARS; 25 mg l(-1) per 6 h) or oxytetracycline hydrochloride (OTC; 200 mg l(-1) per 10 h). The microincrements between fluorescent bands were distinct, ranging from 0·89 to 2·75 µm (mean ± S.D. =1·43 ± 0·28 µm; c.v. = 32%) and from 0·71 to 2·89 µm (1·53 ± 0·27 µm; c.v. = 35%) for ARS and OTC, respectively. The relationship between the number of microincrements between marks and the number of elapsed days for ARS and OCT treatments indicated that there was a significant correspondence between the number of increases observed and the number of days. Hence, daily microincrements of otoliths of E. ringens are likely to be formed in juveniles and adults under natural conditions.

A new spectrofluorimetric method for the determination of some tetracyclines based on their interfering effect on resonance fluorescence energy transfer.

A rapid, simple, inexpensive and highly sensitive spectrofluorimetric method was developed for the determination of trace amounts of some tetracyclines (TCs), namely tetracycline hydrochloride (TCH), oxytetracycline hydrochloride (OTCH) and minocycline hydrochloride (MCH). Binding rhodamine B (RhB) to gold nanoparticles (Au NPs) resulted in quenching of the fluorescence of RhB by a resonance energy transfer (FRET) mechanism, with Au NPs as the energy acceptors. The presence of TCs caused the release of RhB molecules and recovered their fluorescence, and this was used as a basis for the quantitative determination of TCs. The reaction was monitored spectrofluorimetrically by measuring the increase in fluorescence of RhB at 572 nm starting 5 min after mixing the reagents in Tris buffer solution (pH 6.5). The effect of various experimental factors such as buffer type, pH, concentrations of the involved reagents and reaction time were studied to optimize the reaction conditions. Under optimum conditions, the calibration graphs were linear within the ranges 2.08 × 10(-9) -1.04 × 10(-6) mol/L, 2.01 × 10(-9) -1.00 × 10(-6) mol/L and 2.02 × 10(-9) -1.01 × 10(-6) mol/L and detection limits (LODs) of 0.61 × 10(-9) , 0.32 × 10(-9) and 0.66 × 10(-9) mol/L were calculated for TCH, OTCH and MCH, respectively, with corresponding percent relative standard deviations (%RSDs) of 1.18, 1.21 and 1.54 (n = 5). The method was successfully applied to the determination of TCs in drinking water, human urine, bovine milk and breast milk samples.