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Spectrophotometric Method for the Determination of Tetracycline and Doxycycline by Oxidizing Coupling Reaction with 4-aminoantipyrine
... It is occasionally available in ointments to treat skin infections and acne [5]. The determination methods of tetracycline hydrochloride are; spectrophotometric methods [6][7][8][9][10], Chromatographic methods [11][12][13][14][15][16][17] and Electrical methods [18][19][20]. ...
Simple, highly sensitive and accurate spectrophotometric method has been developed to determination of tetracycline hydrochloride in aqueous solution. The proposed method is based on the coupling of tetracycline hydrochloride with 2,4-dinitrophenylhydrazine (2,4-DNPH) in the presence of potassium periodate to form an intense orange color dye at 360nm. Beer’s law is obeyed in the concentration range 0.1-9 μg/ml with the molar absorptivity of 1.262 ×10 ⁴ liter.mol ⁻¹ .cm ⁻¹ , with limit of detection (LOD) of 0.0123μg/ml and limit of quantification (LOQ) of 0.0412μg/ml while the RSD value of 0.184 – 0.467 % depending on the concentration. The proposed method was performed successfully to the determination and analysis of tetracycline hydrochloride in pharmaceutical formulations with average recovery of 100.23 %.
... and proton pump inhibitor in the treatment of peptic ulcer . There have been several analytical methods reported for their determination, both in pharmaceutical formulations and biological samples (fluids and tissues) (Al-Momani and Kanan, 2008;Pourmoslemi et al., 2016;Saber and 2010;Rokayia and Alaa, 2015;, spectrofluorimetry (Attia et al., 2011), Issa et al., 2013;Issa et al., 2016;, TLC (Selvadurai et al., 2012), HPLC ., 2007, capillary electrophoresis et al., 2006), and FIA methods ; Townshend et al., 2005;Palaharn et al., 2003;Rufino et al., 2009). The main goal in the present work and due to the importance of DCH and it's a broad uses, a simple and sensitive spectrophotometric determination for pure and pharmaceutical capsules is involved, which based on the oxidation reaction of the drug with sodium periodate and then coupling with HZD in basic medium to produce an orange color complex at a λ max = 420 ...
In this paper, a novel and sensitive electrochemical aptasensor for detecting tetracycline (TET) with prussian blue (PB) as the label-free signal was fabricated. A PB-chitosan-glutaraldehyde (PB-CS-GA) system acting as the signal indicator was developed to improve the sensitivity of the electrochemical aptasensor. Firstly, the PB-CS-GA was fixed onto the glass carbon electrode surface. Then, colloidal gold nanoparticles (AuNPs) were droped onto the electrode to immobilize the anti-TET aptamer for preparation of the aptasensor. The stepwise assembly process of the aptasensor was characterized by cyclic voltammetry (C-V) and scanning electron microscope (SEM). The target TET captured onto the electrode induced the current response of the electrode due to the non-conducting biomoleculars. Under the optimum operating conditions, the response of differential pulse voltammetry (DPV) was used for detecting the concentration of TET. The proposed aptasensor showed a high sensitivity and a wide linear range of 10−9 ∼ 10−5 M and 10−5 ∼ 10−2 M with the correlation coefficients of 0.994 and 0.992, respectively. The detection limit was 3.2×10−10 M (RSD 4.12%). Due to its rapidity, sensitivity and low cost, the proposed aptasensor could be used as a pre-scanning method in TET determination for the analysis of livestock products.
This paper is a continuation to our previous work aiming at development and validation of a reversed-phase HPLC for modernization of tetracycline-related USP monographs and the USP general chapter <226>. Previous results showed that the method is accurate and precise for the assay of tetracycline hydrochloride and the limit of 4-epianhydrotetracycline impurity in the drug substance and oral suspension monographs. The aim of the current paper is to examine the feasibility of the method for modernization of USP tetracycline hydrochloride capsule monograph. Specificity, linearity, accuracy and precision were examined for tetracycline hydrochloride assay and 4-epianhydrotetracycline limit. The method was linear in the concentration range from 80% to 160% (r>0.9998) of the assay concentration (0.1 mg/mL) for tetracycline hydrochloride and from 50% to 150% (r>0.997) of the acceptance criteria specified in tetracycline hydrochloride capsule monograph for 4-epianhydrotetracycline (NMT 3.0%). The recovery at three concentration levels for tetracycline hydrochloride assay was between 99% and 101% and the RSD from six preparations at the concentration 0.1 mg/mL is less than 0.6%. The recovery for 4-epianhydrotetracycline limit procedure over the concentration range from 50% to 150% is between 96% and 102% with RSD less than 5%. The results met the specified acceptance criteria.
The in vitro activities of doxycycline, chloroquine, quinine, amodiaquine, artemether, pyrimethamine, and cycloguanil were evaluated against Plasmodium falciparum isolates from Senegal (Dielmo and Ndiop), using an isotopic, micro, drug susceptibility test. The 71-50% inhibitory concentration (IC50) values for doxycycline ranged from 0.7 to 108.0 microM and the geometric mean IC50 for the 71 isolates was 11.3 microM (95% confidence interval = 9.5-13.4 microM). The activity of doxycycline did not differ significantly (P = 0.0858) between the chloroquine-susceptible isolates and the chloroquine-resistant isolates. There was no in vitro correlation between the responses to doxycycline and those to artemether, chloroquine, quinine, amodiaquine, pyrimethamine, and cycloguanil, suggesting no in vitro cross-resistance among these drugs. Potency was increased by prolonged exposure. In 96-hr incubations, the activity of doxycycline was 4-5-fold more increased than in 48-hr incubations. The in vitro activity of doxycycline against intraerythrocytic stages of multidrug-resistant P. falciparum, its action against the preerythrocytic forms, the lack of correlation between the responses in vitro of P. falciparum to doxycycline and the other antimalarial drugs, and its original potential site of action are factors that favor its use as antimalarial drug.
An optimized and validated spectrophotometric method has been developed for the determination of Tetracycline hydrochloride (TCH) in pharmaceutical formulations. The method is based on the reaction between TCH, sodium nitroprusside and hydroxylamine hydrochloride in alkaline medium. The product absorbed maximally at 529 nm. Beer's law is obeyed in the working concentration range of 2-60 µg mL-1 with apparent molar absorptivity of 5.049×10 3 L mol-1 cm-1 and Sandell's sensitivity of 0.0952 µg cm 2 / 0.001 absorbance unit. The proposed procedure was applied successfully for estimation of drug in different commercial forms. The proposed method was applied to the determination of the studied drug in pharmaceutical formulations and the results demonstrated that the method is equally accurate and precise as the official method as found from the t-and F-values.
For the determination of trace residues of tetracycline antibiotics in fatty food samples, selective pressurized liquid extraction coupled with high-performance liquid chromatography and tandem mass spectrometry was applied in this paper. Copper(II) isonicotinate was first used as online cleanup adsorbent in SPLE process. The adsorbent to sample ratio, extraction temperature, extraction time, and recycle times, etc. were optimized. The tetracyclines in food samples of pork, chicken meat and clam meat were detected by liquid chromatography with tandem mass spectrometry. Tetracycline was found at levels of 0.32 and 0.53 μg g−1 and oxytetracycline was found at 0.14 and 0.21 μg g−1 in chicken meat and clam meat, respectively, while chlorotetracycline and deoxytetracycline were below the detection limit. The detection limit (S/N = 3) for these four tetracyclines were from 0.2 to 3.3 ng g−1, the recoveries were from 75.8 to 110.5%, and relative standard deviations were from 5.5 to 13.6%. Copper(II) isonicotinate showed a higher purification capacity than other cleanup adsorbents for extraction of antibiotics in fatty food, and the recovery showed predominance compared with a pressurized liquid extraction method without adsorbent. The study demonstrated that copper(II) isonicotinate would be a promising cleanup adsorbent in pressurized liquid extraction for the analysis of trace organic pollutants in complicated samples.This article is protected by copyright. All rights reserved
A novel reversed-phase HPLC method was developed and validated for the assay of tetracycline hydrochloride and the limit of 4-epianhydrotetracycline hydrochloride impurity in tetracycline hydrochloride commercial bulk and pharmaceutical products. The method employed L1 (3 µm, 150 × 4.6 mm) columns, a mobile phase of 0.1% phosphoric acid and acetonitrile at a flow rate of 1.0 mL/min, and detection at 280 nm. The separation was performed in HPLC gradient mode. Forced degradation studies showed that tetracycline eluted as a spectrally pure peak and was well resolved from its degradation products. The fast degradation of tetracycline hydrochloride and 4-epianhydrotetracycline hydrochloride in solution was retarded by controlling the autosampler temperature at 4 °C and using 0.1% H3 PO4 as diluent. The robustness of the method was tested starting with the maximum variations allowed in the US Pharmacopeia (USP) general chapter Chromatography <621>. The method was linear over the range 80-120% of the assay concentration (0.1 mg/mL) for tetracycline hydrochloride and 50-150% of the acceptance criteria specified in the individual USP monographs for 4-epianhydrotetracycline hydrochloride. The limit of quantification for 4-epianhydrotetracycline hydrochloride was 0.1 µg/mL, 20 times lower than the acceptance criteria. The method was specific, precise, accurate and robust. Copyright © 2014 John Wiley & Sons, Ltd.
Developing the rapid, simple and sensitive biosensor system for tetracycline detection is very important in food safety. In this paper, we developed a label-free aptasensor for electrochemical detection of tetracycline. The reorganization of tetracycline binding aptamer was confirmed by Isothermal Titration Calorimetry, Kd = 5.18 × 10−5 mol L−1. According to the electrochemical impendence spectroscopy (EIS) analysis, there was a linear relationship between the log concentration of tetracycline and the charge transfer resistance (ΔRet) from 5.0 to 5.0 × 103 ng mL−1 of the tetracycline conc. The detection limit was 1.0 ng mL−1 within a detection time of 15 min. The average of assemble rate Q was at 82.4% with a differential batches' RSD of 4.6%. The current change of this aptasensor lies within at 8.5% after a storage of 15 days under 4 °C. The result aptasensor had shown a good reproducibility with an acceptable stability in tetracycline detection. The recoveries of TET in spiked milk samples were in the range of 90.0–95.7%.
A sensitive analytical method for determination of doxycycline (DC) residues in chicken fat/fat and skin was developed. The extraction, in the presence of the internal standard (IS) minocycline (MINO), was carried out using solution of oxalic acid (pH 4.0) and ethyl acetate. The samples were cleaned up by solid phase extraction (SPE) procedure using, at first carboxylic acid and then polymeric Strata X cartridges. Chromatographic separation of DC by LC-UV was achieved on a Luna C8 analytical column and for LC-MS/MS analysis Luna C18 column was used. The presented procedures were evaluated according to the Commission Decision 2002/657/EC. Specificity, decision limit (CCα), detection capacity (CCβ), recovery (absolute and relative), precision (repeatability and reproducibility) were determined during validation process. The limit of detection (LOD) was 10μg/kg for LC-UV and 1μg/kg for LC-MS/MS method. The limit of quantitation (LOQ) was 15 and 2μg/kg for LC-UV and LC-MS/MS, respectively. The absolute recovery for the LC-UV and relative recovery for the LC-MS/MS method at 300μg/kg concentration level were 79%; 101% for fat and 82%; 99% for fat and skin, respectively. The developed liquid chromatography with ultraviolet detection (LC-UV) and liquid chromatography tandem mass spectrometry (LC-MS/MS) methods have been applied to quantitative determination of doxycycline (DC) in samples of chicken fat tissue obtained from animals treated with DC.
The new simple, cost effective and well performing differential pulse stripping voltammetry method for the simultaneous determination of antibiotics – oxytetracycline, tetracycline and chlorotetracycline was researched and developed. It depends on the reduction of these compounds at a hanging mercury drop electrode. The samples were extracted from (i) spiked animal feed, and (ii) fresh fish muscle dosed with the drugs. The voltammograms from the drug mixture produced complex, overlapping profiles, and chemometrics methods were applied for calibration modelling. The analytical linear ranges were within 0.02–0.18 μg mL−1 and the corresponding LODs were 3–5 μg L−1 for the three analytes. These values compare well with those from the HPLC and fluorescence methods in the literature. The % relative prediction errors from the verification trials were between 4% and 9% with % Recoveries being 103–107. Also, the % Recoveries of the antibiotics from animal feeds as measured by the new method were comparable with those from the HPLC analysis (85%), i.e. the method is highly competitive, especially as a screening approach.
The Complete Drug Reference
- Martindale
Martindale, (2009), "The Complete Drug Reference". 36th ed. London: Pharmaceutical Press,
257-659.
Spectrophotometric Determination of Tetracyclines using P-N,N-Dimethyl Phenylene Diamen and Sodium Metaperiodate
- E D Tella
- M Taherunnisa
- G K Deepthi
- B M Choragudi
- C B Ranjani
Tella, E. D.; Taherunnisa, M.; Deepthi, G.K.; Choragudi, B. M. and Ranjani C. B., (2011),
"Spectrophotometric Determination of Tetracyclines using P-N,N-Dimethyl Phenylene Diamen
and Sodium Metaperiodate" Rasayan J. Chem., 4, 3, 539-543 ISSN: 0974-1496.