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Aminoglycosides are antimicrobial agents used frequently in treatment of human and animal diseases caused by aerobic, gram-negative bacteria. Because of the toxicity of these compounds, considerable effort has been attributed to analysis of aminoglycoside content in drug preparations, in serum and urine specimen in therapeutic drug monitoring, and...
Citations
... Kanamycin (KAN) belonging to the type of aminoglycoside antibiotics has been extensively used in food production and veterinary drug [1][2][3], and can be used in treating infectious diseases caused by Gram-negative and Gram-positive [4] on account of a strong inhibitory effect on bacterial infections [5]. KAN that remains in food and environment can enter human body by means of food chain, such as honey products, milk products, and lake water, and then threaten human health furthermore [6][7][8]. ...
Based on fluorescence resonance energy transfer, an ultrasensitive aptasensor was designed to detect kanamycin. Carbon quantum dots (CQDs) connected to the 3′ end of the hairpin aptamer (HP) acted as energy donor, while gold nanoparticles (AuNPs) bound to the 5′ end of HP acted as energy acceptor. The interaction due to the overlapping between absorption spectrum of AuNPs and emission spectrum of CQDs led to an obvious quenching. After adding kanamycin, the specific binding between target and HP made the HP structure change. Then, the distance between CQDs and AuNPs increased gradually, and fluorescence intensity would recover. Therefore, the recovery of fluorescence intensity can be used for kanamycin detection via optical responses. Under optimal conditions, fluorescence intensity had a good linear relationship with the logarithm of kanamycin concentration. The detection limit of kanamycin was 5.7 pM (3.22 × 10–3 μg/kg) and the detection concentration of kanamycin concentration was 0.01–500 nM (5.65 × 10–3–282.80 μg/kg). The aptasensor was also applied into the determination of kanamycin residues in milk.
... It is widely used to treat Gram-negative infections, particularly against species of Pseudomonas aeruginosa [13]. Tobramycin was discovered by Eli Lilly in 1967 [14] and is effective by interrupting ribosomal cell functions [15,16]. For medical use, tobramycin is typically used in eye drops (ophthalmic solutions) (at 0.3%(w/v)) for treatment of eye infections [17][18][19]. ...
The analysis of tobramycin was demonstrated successfully as an example for electrospray ionization on an open-source hardware ion mobility spectrometer. This instrument was assembled inexpensively in-house, and required only very few purpose-made components. The quantitative determination of tobramycin required 20 s for a reading. The calibration curve for the range from 50 to 200 μM was found to be linear with a correlation coefficient of r = 0.9994. A good reproducibility was obtained (3% relative standard deviation) and the limit of detection was determined as 8 μM. As the concentration of the active ingredient in the eye drops (ophthalmic solutions) is too high for the sensitivity of the instrument, the samples had to be diluted appropriately.
Graphical abstract
... In addition, it has been reported that the time required for pretreatment is long, and reproducibility is low [5][6]8]. In particular, it has been reported that aminoglycoside-based components are challenging to analyze using GLC without the derivatization of amino and hydroxyl groups due to the hydrophilicity and non-volatile nature of the molecule [9]. ...
This study developed a suitable analytical method for kasugamycin residues in Achyranthes japonica using LC/MS/MS equipped with an amide column for polar substances. Extraction and cleanup processes were done at pH 4.5–5. Purification efficiency was assessed and confirmed step by step by selecting silica, hydrophilic-lipophilic balance (HLB), strong cation exchange (SCX), and double (HLB and SCX) cleanup SPE cartridges. The results indicated that silica SPE cartridge exhibited overloading tendency, while HLB SPE cartridge had low cleaning efficiency. Among SPE cartridges used, double cleanup and SCX were found sufficient with respective matrix effects of –15% and +14%, respectively. The LOD and LOQ were 0.008 ng and 0.04 mg/kg, respectively. The correlation coefficient (R2) was higher than 0.99, recovery rate ranges were 86.3–97.2%, and the RSD was below 8.8%. All methods are consistent with the Codex guidelines criteria. This study developed an appropriate LC/MS/MS analytical method for kasugamycin residue analysis in A. japonica with optimized, efficient extraction and purification conditions using a single SCX SPE cartridge, which is simple and time-efficient. In addition, the HLB and SCX SPE cartridges of the double cleanup methods were identified as primary methods that can be applied for the cleanup of other medicinal herbs.
... GEN plasma levels are usually measured using immunochemical methods [4]. The use of liquid chromatographic (LC) methods for GEN measurement in biofluids pose some challenges, particularly due to its high hydrophilicity and lack of chromophores [5,6]. More recently, the use of LC associated to mass spectrometry (LC-MS/MS) has become a method of choice for drug measurements in the context of TDM. ...
Background
Therapeutic drug monitoring (TDM) of gentamicin sulfate (GEN) is usually recommended, particularly in critical patients. Only a few reports had described the determination of GEN in plasma or plasma using LC-MS/MS.
Objective
This study aimed to develop and validate a sensitive ultra-high-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) assay for the quantification of GEN in small volumes of human plasma.
Results
The use of a very low concentration of the ion-pairing agent HFBA allowed significant retention of the very polar GEN forms in a reversed phase UHPLC column. The solid-phase extraction (SPE) procedure allowed clean extracts, with no interferences detected in blank samples, and high sensitivity. The assay was linear on the range of 0.2–40 mg L⁻¹ of GEN complex. The combined GEN complex had inter-assay CV of 8.8–10.0%, intra-assay CV of 10.2–11.0%, and accuracy of 96.8–104.0%. The assay was applied to 17 clinical samples obtained from neonate patients. Measured concentrations were in the range of 0.15–3.57 mg L⁻¹ for GEN C1, 0.12–3.55 mg L⁻¹ for GEN C1a, 0.20–5.77 mg L⁻¹ for GEN C2, and 0.47–12.88 mg L⁻¹ for the GEN complex, all within the linear range of the assay.
Conclusion
A sensitive assay for the quantification of gentamicin in plasma using anion-exchange SPE and UHPLC-MS/MS was validated. The assay can be used for TDM of gentamicin, particularly in centers with access to proper instrumentation and with a low demand for gentamicin measurements, where immunoassays are not cost-effective.
... To date, reviews and discussion cover AmG antibiotics in general and not TBM specifically. Some analytical methods for quantifying TBM were reported in a general review on chromatographic methods for the analysis of AmG antibiotics [37]. In 2015, challenges associated with different matrices were discussed for analyzing AmG [38]. ...
... RI is a non-destructive detector, widely used in the analysis of compounds that do not absorb in UV-Vis, such as analytes derived from carbohydrates and AmGs [2,37]. However, its main disadvantage is that it is sensitive to changes in pressure and temperature, which is incompatible with protocols that involve an elution gradient. ...
Tobramycin (TBM) is an aminoglycoside antibiotic mostly used for infections caused by gram-positive although it can be indicated for some gram-negative organisms. Due to the absence of chromophore groups in TBM and its basicity, several different analytical approaches have been described in the literature for its quantification using HPLC that address specific aspects of its physical–chemical properties. Some methods are based on derivatization with chromophores and fluorescence molecules. Others apply techniques for detection such as mass spectrometry, electrochemical pulse detector, amperometric pulse detection, refractive index and evaporative light scattering. There are also approaches to the separation that include capillary and micellar electrophoresis. The applicability of different types of detectors in the quantification of TBM, along with its degradation products, are discussed to present advantages and disadvantages as well as the use of ion pairs and different stationary phases.
... Several analytical methods have been developed for the determination of KAN from food samples such as high-performance liquid chromatography, gas chromatography, and mass spectrometry still being the gold standards [9,10]. Moreover, simple and fast detection of KAN has also been reported in the literature using colorimetric [11], fluorometric [8,12], enzyme-linked immunosorbent analysis [13], surface plasmon resonance (SPR) [5], and electrochemical-based [14,15] detection strategies. ...
In this work, molecularly imprinted kanamycin (KAN) electrodes were prepared using electrochemical polymerization of pyrrole (Py). First, a glassy carbon electrode was coated with an optimized volume of graphene oxide (GC/GO) to provide a high surface area electrode. Py is then polymerized on GC/GO electrode using cyclic voltammetry in the presence of KAN following by KAN removal using HCl (GC/GO-pPy-KAN*). Electrode preparation steps were also optimized using microscopic, spectroscopic, and electrochemical methods. Finally, the analytical performance of the prepared GC/GO-pPy-KAN* electrode was investigated for the determination of KAN. The limit of detection and the detection range was calculated as 5 nM and 5 nM–1 µM, respectively. The precision, accuracy, and interference studies showed good precision and relative error with minimum interference for the chosen substances. Moreover, real sample analysis was also performed using 4 different milk samples with good recovery values. Consequently, a novel, simple, and sensitive sensor was developed using an easy and low-cost fabrication method for the detection of KAN in food samples such as milk.
... Immunological methods such as enzymatic assay (EA) and radioimmunoassay (RIA), despite their great sensitivity, specificity and high throughput capability in the analysis of AMGs, suffer from drawbacks such as suppression of enzymes activities due to environmental factors, special equipment, radioactive materials and skilled technicians [8][9][10] . Reversed-phase HPLC is the most https://doi.org/10.1016/j.chroma.2020.461343 ...
A simple magnetic dispersive solid-phase extraction (MDSPE) methodology based on mesoporous Fe3O4@ succinic acid nanospheres and high‐performance liquid chromatography–tandem mass spectrometry (HPLC‐MS/MS) has been developed to determine kanamycin (KNM) and neomycin (NEO) contents in Measles, Mumps, and Rubella (MMR) vaccine products. The monodispersed mesoporous Fe3O4 nanospheres with self-assembled carboxyl terminated shell have been prepared via a simple solvothermal method. These as-synthesized mesoporous Fe3O4 nanospheres showed a high magnetic saturation value (Ms = 46 emu g⁻¹) and large specific surface area (111.12 m² g⁻¹) which made them potential candidates as sorbents in magnetic solid-phase extraction. The adsorption experimental data fitted well with the Freundlich-Langmuir isotherm and followed a pseudo-second-order kinetic model. Moreover influential parameters on extraction efficiency were investigated and optimized. Under optimal conditions, the limits of detection for KNM and NEO were 1.0 and 0.1 ng mL⁻¹, respectively. Recovery assessments using real samples exhibited recoveries in the range of 96.0 ± 4.3 to 101.5 ± 7.1 %, with relative standard deviations of <10.7% (for intra- day) and <14.6% (for inter- day). The proposed method was successfully applied for different spiked and un-spiked MMR vaccine samples. The presented extraction method provides a fast, selective, robust and practical platform for the detection of KNM and NEO in MMR vaccine samples.
... Change in current flow is occurred due to oxidation of the analyte at the surface of an electrode, therefore chromatograms achieved by plotting current against time. AGSs residues have been detected by carbon paste and gold electrodes [118] . ...
Antibiotics, a class of inexpensive broad-spectrum medicine service in treating animal infectious disease and promoting growth. In recent years, driven by economic interest, antibiotic-resistant has been considered as a significant public health concern, due to the growing appearance of strains of bacteria resistant to antibiotics. The overuse of antibiotics can result in losing their effectiveness to kill bacteria which leads to the difficulty of treating diseases due to the new generation of bacteria have genes with resistance to some antibiotics. Therefore, the continuous application of antibiotic in animal husbandry can lead to an accumulation of resistant bacteria in the food of animal origin which causes illnesses that are difficult to treat. Besides antibiotic-resistant, the overuse of antibiotic can occur in several diseases including liver damage, ototoxicity, nephrotoxicity, allergic reactions, and yellowish discoloration of teeth. Subsequently, the World Health Organization (WHO) has considered antibiotic as one of the international concern due to the highest health risk to humanity. Henceforward, WHO has recognized the acceptable daily intake (ADI) and the maximum residue limit (MRL) to control antibiotic residues in the food of animal origin and environment.
Up to now, the commonly used antibiotic detection methods mainly include high-performance liquid chromatography, electrophoresis, electrochemical analysis, and microbiological techniques. Although the above methods have high sensitivity, low detection limit, and high accuracy, however, the instruments used are expensive and require a particular operation. Besides, the sample preparation process is complicated and cumbersome, time-consuming, and it cannot be universally promoted, and it is unable to meet the detection requirements of a large number of samples on-site. On the other hand, colorimetric sensors are the most promising for antibiotic detection technology because of their advantages such as simple operation, detection can be achieved directly by naked eye observation, low cost, small size, good selectivity, and no need for expensive instruments. Therefore, researchers have conducted much research on the colorimetric detection of antibiotic from liquid and solid phases. However, existing liquid antibiotic detection systems generally have problems such as insufficient anti-interference ability, harsh storage conditions, and poor portability. Although the solid phase system improves portability and stability to a certain extent, the obtained colorimetric sensor still has low sensitivity, and the naked eye detection limit cannot meet the actual application requirements.
In this thesis, systematic research and exploration are carried out on the above vital issues. Based on the high specific surface area, good pore structure and controllable bulk density of electrospun nanofiber membranes, the antibiotic colorimetric sensors based on electrospun nanofibers were proposed for the first time. The design and construction of the colorimetric sensor can fill the blank of the electrospinning nanofiber material in the research field of antibiotic sensor application. The main research results obtained are summarized as follows:
（1） A fast-response and reusable oxytetracycline colorimetric sensing system was prepared by immobilization of nickel (II) ions on carboxymethylcellulose (CMC) coated polyacrylonitrile nanofibrous membranes (PAN NFMs). Firstly, PAN NFMs were successfully prepared by using electrospinning technology with a specific surface area of 11.39 m2g-1. Then CMC was coated on the PAN NFMs (CMC/PAN). The coated PAN NFMs surface was a suitable platform to achieve effective immobilization of the nickel (II) ions. Due to the strong-complex behavior between nickel (II) ions and oxytetracycline, the constructed sensing platform has shown a colorimetric signal response from light green to yellow toward oxytetracycline, with a naked eye limit of 5 nM at S/N = 3, rapid response (2 min), good reversibility (10 cycles) and selectivity.
（2） Motivated by the nickel ions (Ni2+) colorimetric based system and according to the pharmacological theory, iron ions (Fe3+) and copper ions (Cu2+) can also strongly complex with tetracycline (TC) owing to numerous O- and N-containing groups. Therefore, the impact of such colorimetric sensing system was studied to improve the sensitivity and naked eye detection limit in this part. A strategy to prepare free-standing, nanofibrous structured test strips with tortuous porous structure and large surface area by combining PAN NFMs, sodium alginate, and Fe3+ was presented. Besides, Cu2+ impregnated strips with the nanofibrous structure using ethylenediamine (EDA) grafted porous PAN (EPAN) was also presented. To construct tetracycline (TC)-sensing surface alginate was used to functionalize the PAN NFMs firstly, then Fe3+ were assembled into alginate surface (FAPAN). On the other hand, porous PAN NFMs were modified by ethylenediamine (EDA) firstly, then Cu2+ were immobilized on NFMs to construct another TC-sensing surface (CEPAN). The resultant FAPAN test strips exhibit the integrated properties of fast sensing process (10 min), low naked eye detection limit (5 µg/kg at S/N = 3), excellent anti-interference ability, and certain reusability. Furthermore, the TC concentration-dependent color change (yellow to maroon) were quantitatively visualized by an iPhone read-outed hue parameter. However, the CEPAN colorimetric system has not shown any color response toward TC, because the nanofibers and TC have the same chemical groups which are coordinated with copper ions.
（3） In addition, compared with metals ions, AuNPs have recognized as an excellent agent for the developments of colorimetric sensors due to the ease of preparation, high molar absorptivity, high surface area, biocompatibility, and uniform shape and size; which make them have higher extinction coefficients than metals ions. Therefore, the non-enzymic melamine-AuNPs (MA@Au) conjugated probe system was also developed and applied for colorimetric detection of metronidazole (MTZ). Firstly, AuNPs with an average diameter of 20.1±1.76 nm were successfully prepared by using sodium citrate reduction method with HAuCl4. The non-enzymic MA@AuNPs probe was successfully developed by conjugation of the melamine with AuNPs. The polyamide (PA6) nanofibers membrane was prepared by electrospinning technology. Then the non-enzymic (MA@Au) was immobilized on the PA6 NFMs. The sensing performance showed a colorimetric response to detect metronidazole, with low necked eye limit of detection (2 nM at S/N = 3), a rapid detection time (2.5 min) and linear response in the 2 to 100 nM MTZ concentration range.
（4） Furthermore, aptamers are synthetic biomolecules that can be suggested as a sensing agent to detect any type of antibiotics, due to high affinity and specificity bind to a specific target. Here, kanamycin (KMC) was selected as a representative target antibiotic agent, and a non-aggregated aptamer-AuNPs bio-conjugates probe system was proposed. The KMC-responsive aptamer was used as a response element to improve the selectivity of the system. The selected colorimetric agent was AuNPs with an average particle size of 17.5 nm synthesized using sodium citrate reduction method. The non-aggregated AuNPs probe was successfully prepared by bio-conjugation of kanamycin-responsive aptamer with AuNPs. The probe-supported platform was selected as glutamic acid grafted electrospun cellulose acetate (CA) nanofiber membrane (G-CA NFMs). The carboxylic acid groups on the NFMs surface were acquired, which is an order of the effective immobilization of the Apt@Au probe is achieved, which was constructed a sandwich structured sensing platform. Subsequent sensing performance has shown a colorimetric signal response to kanamycin, due to Apt@Au conjugates disassembly. The biosensor strips displayed high sensitivity for KMC determination in a range 2.5~80 nM, with a naked eye limit of 2.5 nM at S/N = 3. In addition to the excellent selectivity, reusability, and long-term storability, the strips also can be applied in real samples detection.
... Kanamycin was isolated in 1957 [8]. It is a mixture of several closely related compounds, such as main constituent kanamycin A (>95%), as well as minor constituents kanamycin B, C, and D (<5%). ...
Kanamycin is an aminoglycoside antibiotic widely used in treating animal diseases caused by Gram-negative and Gram-positive infections. Kanamycin has a relatively narrow therapeutic index, and can accumulate in the human body through the food chain. The abuse of kanamycin can have serious side-effects. Therefore, it was necessary to develop a sensitive and selective analysis method to detect kanamycin residue in food to ensure public health. There are many analytical methods to determine kanamycin concentration, among which high performance liquid chromatography (HPLC) is a common and practical tool. This paper presents a review of the application of HPLC analysis of kanamycin in different sample matrices. The different detectors coupled with HPLC, including Ultraviolet (UV)/Fluorescence, Evaporative Light Scattering Detector (ELSD)/Pulsed Electrochemical Detection (PED), and Mass Spectrometry, are discussed. Meanwhile, the strengths and weaknesses of each method are compared. The pre-treatment methods of food samples, including protein precipitation, liquid-liquid extraction (LLE), and solid-phase extraction (SPE) are also summarized in this paper.
... Various methods have been reported for analysis of cefepime (Spectrophotometry: Rambabu, Jyothirmayee, Naga Raju, 2012;Elazazy, Shalaby, 2012;Khare et al., 2012;Sujith, Abraham, Divakar, 2010;Nanda et al., 2012;Chafle, 2013;El-Shanawany et al., 2014;Patel et al., 2015a;Papanna, Krishnegowda, Nagaraja, 2015;Kant et al., 2015;Bhupendra, Bhuyan, Sinha, 2011;Chromatography: Sunitha et al., 2013;Dave Vimal, 2012;Patil et al., 2012;Khan, Iqbal, Khattak, 2012;Medina et al., 2007;Patel et al. 2010;Panchal Vipul et al., 2014;Ashok,Veenaeesh, Siripurapu, 2013;Syama Sundar, Gurucharana Das, 2014;Bhavana et al., 2013;Abdel-Aziz et al., 2014;Mughal et al., 2016;Chromatography: Sunitha et al., 2013;Dave Vimal, 2012;Patil et al., 2012;Ramakrishna et al., 2014;Behan, Punitha, Krishanan, 2013;Khan, Iqbal, Khattak, 2012;Medina et al., 2007;Patel et al., 2010;Neelima et al., 2013;Patel et al., 2015b;Baririan et al., 2003;Panchal Vipul et al., 2014;Ashok et al., 2013;Syamsundar, Guruchana Das, 2014;Arayne, Sulthana, Nawaz, 2006;Bhavana et al., 2013;Trivedi, Kshtri, Patel, 2013;Abdel-Aziz et al., 2014) and along with other combination of drugs and few analytical methods have been reported with the amikacin drug (Spectrophotometry: Mugal et al., 2016;Omar et al., 2013;Soltés, 1999, Omara, Amin, 2013Ryan, 1984;Chromatography: Feng, et al., 2001;Mokh et al., 2014;Isoherranen, Soback, 1999;Bhatt et al., 2015). But there is only one spectrophotometry method reported for the analysis of both cefepime and amikacin in combination (Kalyani, Rao, 2016). ...
A simple, accurate, isocratic stability indicating RP-HPLC method was developed for the determination of cefepime and amikacin in Pure and its pharmaceutical formulations. The method consists of methanol: acetonitrile:acetate buffer 75:20:05 (v/v) mobile phase at pH 5.1 with C18 column as stationary phase. The flow rate and detection wave length were 1.0 mL/min and 212 nm respectively. The linearity range for the method was found to be 2.5-25 µg/mL for amikacin and 10-100 µg/mL cefepime respectively. The developed method was validated as per ICH guidelines and the results of all the validation parameters were well within their acceptance values. Also the forced degradation studies were conducted with standard drugs. Degradation products formed during the different stress conditions were separated from both drugs. This validated method was applied for the simultaneous estimation of cefepime and amikacin in commercially available formulation sample.
