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Electrospray ionization mass spectra (ESI-MS) of kasugamycin-HCl salt (MW = 433.8) dissolved in water. The base peaks at m/z 380.1 and 402.1 corresponding to the (M+H) + and (M+Na) + ions of kasugamycin (MW = 379.4), respectively.
Source publication
A high performance liquid chromatographic (HPLC) analysis method with an ultraviolet (UV) detector and an Aqua C18 (250 x 4.6 mm, Phenomenex) column were applied to analyze the antibiotic fungicide kasugamycin in water. An aromatic sulfonic acid spe column (Backerbond, J. T. Backer) was used to remove the interfering materials from irrigation water...
Citations
... KASU was reported to reveal a considerable thermal instability, is non-volatile and exhibits amphoteric properties combined with extremely high hydrophilicity (Fan, Guo, Liang, Dong, Ding, Zhang, Tang, Yang, Kong, & Cao, 2017). Additionally, it is unstable in alkaline medium even at ambient temperature and lacks any characteristic ultraviolet absorption spectrum (Sheu, Chen, & Lo, 2010). These complex physico-chemical properties of KASU hinder its detection using commonly applied spectrophotometric or UV based HPLC detection approaches. ...
... These complex physico-chemical properties of KASU hinder its detection using commonly applied spectrophotometric or UV based HPLC detection approaches. Capillary electrophoresis (Lo & Hsiao, 1996) and liquid chromatography (LC) equipped with ultraviolet detector (Sheu, Chen, & Lo, 2010) have been employed for KASU detection in various samples. Unfortunately, as a result of non-characteristic ultraviolet absorption of KASU, the detection wavelength was set at 210 nm which in turn would affect the accuracy and sensitivity of the method due spectral interference (Li, Dai, Pu, Bian, Chen, Zhang, Guo, Li, Li, Yong, Wang, Zhang, & Han, 2020). ...
Kasugamycin residues (KASU), a pest control antibiotic, was reported as an ecosystem threat owing to its over-application in plant protection to meet the growing global need for agronomic products. Therefore, we report herein the first electrochemical sensor for fast and sensitive analysis of KASU in vegetables based on the synergetic hybridization between conducting polyserine film (poly (SER)), and carbon nanomaterials including functionalized multiwalled carbon nanotubes (fMWCNTs) and reduced graphene oxide (rGO). The sensor was characterized morphologically using Scanning electron (SEM) and atomic force Microscopy (AFM), while cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) were used for electrochemical characterization. Under the optimized conditions using differential pulse voltammetry (DPV), the sensor exhibited an outstanding sensitivity and selectivity, with a good linear response of 3-106 µg/mL and an assessed limit of detection and quantification of 0.40 and 1.33 µg/mL, respectively. Furthermore, the electrochemical sensor was effectively applied to quantify KASU in cucumber, zucchini, and carrots with a recovery range 95.5-100.1%, and RSD lower than 4.1% (n = 3), showing its applicability and efficiency for selective analysis of KASU in foodstuffs.
... Kasugamycin and rifamycin resistance genes were present in all rainfall runoff samples but not in the CSO outfall. Kasugamycin is usually used as agricultural insecticide (Sheu et al. 2010), and rifamycin is usually used for the treatment of tuberculosis (Adams et al. 2021). These two antibiotics were not the common drugs in urban life. ...
Rainfall runoff and combined sewer overflow (CSO) converge with organic waste, nutrients, and microbes from the ground and wastewater. These pollutants promote the spread and transformation of antibiotic resistance genes (ARGs). In this study, four rainfall runoff and one CSO outfall were chosen, and samples were collected to explore the occurrence and distribution of ARGs. The ARGs were extracted from suspended solids and analyzed using metagenomic sequencing. A total of 888 ARG subtypes, belonging to 17 ARG types, were detected in all samples. Eleven ARG types were shared by all the samples. Multidrug resistance genes had the highest relative abundance. Their total relative abundance reached 1.07 ratio (ARG copy number/16S rRNA gene copy number) and comprised 46.6% of all the ARGs. In all samples, the CSO outfall had the highest total relative abundance (8.25 × 10−1 ratio) of ARGs, with a ratio ranging ND (not detected)–3.78 × 10−1 ratio. Furthermore, the relationship between ARG types and environmental factors was determined using redundancy analysis. The results showed that chemical organic demand (COD) and bacterial abundance were positively correlated with most ARG types, including multidrug, bacitracin, aminoglycoside, β-lactam, tetracycline, and sulfonamide. NH3-N, TN, and TP were positively correlated with rifamycin, fosmidomycin, and vancomycin resistance genes. The relationship among the ARG subtypes was investigated using network analyses. The multidrug resistance gene subtypes had the highest frequency of co-occurrence. This study provides insights into the occurrence and distribution of ARGs under non-point source pollution and may contribute to the control of ARGs.
... Kasugamycin was detected by using the HPLC method referenced from Ceshing Sheu with improvement. 31 Briefly, the mobile phase consisted of eluent A, acetonitrile, and eluent B, water with 0.1% H 3 PO 4 and 0.1% sodium dodecyl sulfate (SDS) (40:60 v/v). An analytical C 18 ODS column (250 mm × 4.6 mm, 5 μm; DIKMA, Beijing, China) was equipped with a guard column (4 mm × 3 mm) and pre-equilibrated with the mobile phase for about 40 min before analysis. ...
The controlled and targeted release of pesticides with high water solubility has been a challenge for integrated pest management. In this paper, kasugamycin, an antibiotic broadly used in plant disease controlling, was covalently conjugated to pectin to form a kasugamycin-pectin conjugate by an amide bond. The conjugate was structurally characterized by fourier transform infrared spectroscopy, ultraviolet spectrophotometer and thermal gravimetric analysis. The results showed that the conjugate was stable at a wide range of pH and temperatures, as well as under UV irradiation. When incubated with Pseudomonas syringae pv. Lachrymans, the conjugate could be activated with releasing the kasugamycin, which made it a promising controlled release formulation of pesticide.
... L. Lu e-mail: luleibendan@126.com water by HPLC (Sheu et al. 2010). Despite these studies, no development of the fate of kasugamycin during degradation in chilli fields has been observed. ...
A simple and efficient method for determination of kasugamycin in chilli and soil was developed, and the fate of kasugamycin in chilli field ecosystem was also studied. Kasugamycin residues were extracted from sample, cleaned up by solid phase extraction and chromatographic column and then determined by ultra performance liquid chromatography with tandem mass spectrometry detection. The method got recoveries ranged from 77.82% to 83.35% with relative standard deviations of 2.20%-6.54%. As far as the accuracy and precision was concerned, the method met certain standard. The LODs of kasugamycin calculated as a sample concentration (S/N ratio of 3) was 2.50 μg kg(-1). The degradation of kasugamycin in chilli and soil was determined. The results showed that kasugamycin degradation in chilli plant and soil followed the first-order kinetics. The half-lives of kasugamycin in chilli and soil was 2.76-3.77 and 3.07-3.91 days, respectively. The final kasugamycin residues in chilli and soil were undetectable at levels of recommended and 1.5 times recommended dosage with an interval of 21 days.
An ultrahigh-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established for the determination of four highly polar agricultural antibiotics kasugamycin, validamycin A, ningnanmycin, and polyoxin B in plant-derived foods. The samples were extracted with a 0.2% formic acid solution, purified by hydrophilic-lipophilic balance and mixed-mode cation-exchange solid-phase extraction, and then reconstituted for UPLC-MS/MS detection. The chromatographic analysis was performed on a BEH Amide column (100 mm × 2.1 mm, 1.7 μm) using gradient elution with a 0.1% formic acid solution and 0.1% formic acid acetonitrile as mobile phases. Method validation was performed on 15 matrices spiked at 0.02 (or 0.05), 0.5, and 2 mg/kg. The mean recovery rate ranged from 75 to 102% with relative standard deviations (RSD) was less than 20%. Good linearities (r > 0.99) in the range of 0.002-0.2 μg/mL were obtained. The limits of quantification (LOQs) were 0.02 and 0.05 mg/kg. Studies on the stability of the analytes in the stored kiwifruit samples showed that kasugamycin, validamycin A, and ningnanmycin were stable for at least 6 months, while polyoxin B was observed to be partially degraded (the degradation rate at 6 months was 31.3%). The method was demonstrated to be effective and reliable in real samples. In the kiwifruit samples treated after 7 days, no residues of ningnanmycin and polyoxin B were detected, while the residues of kasugamycin and validamycin A were 0.12 and 0.038 mg/kg, respectively.
Two polar aminoglycosides, kasugamycin and validamycin-A were determined in cereals (brown rice, wheat and corn) by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The analytes were extracted from samples using methanol and water (70:30, v/v) at pH 5.5, purified using both a hydrophilic-hydrophobic-balanced (HLB) cartridge and strong cation exchange (SCX) cartridge, and then analyzed using multiple reaction monitoring (MRM) in positive electrospray ionization mode with a special ReproSil 100 C18 HPLC column. This newly proposed method gave good sensitivity and excellent chromatographic performance. The limits of quantification (LOQ) for kasugamycin and validamycin-A were 4.1 µg/kg and 1.0 µg/kg, respectively. The recoveries for both compounds at three fortification levels (4, 100 and 500 µg/kg for kasugamycin; 1, 10 and 100 µg/kg for validamycin-A) ranged from 75% to 110%, and the relative standard deviations were below 15%.
A lateral flow strip biosensor for fast, sensitive, low-cost and on-site detection of kanamycin was developed by using kanamycin-specific aptamer-modified gold nanoparticles (AuNPs-apt) as probe and oligonucleotide DNA1-modified silver nanoparticles (AgNPs-DNA1) as signal amplification element. Through the complementary sequences of DNA1 and the aptamer, AgNPs-DNA1-apt-AuNPs complex can be formed and further captured on the test zone of the strip, where a capture probe DNA2 complementary to 3’-terminal of DNA1 was immobilized. The presence of kanamycin can competitively bind to the aptamer, then inhibit the formation of the complex and the accumulation of AuNPs on the test zone. AuNPs-apt can finally be captured on the control zone via the specific binding between biotin and streptavidin. The assay avoids the multiple incubation and washing steps, and can be completed within 10 min. By observing the color change of the test zone, a qualitative detection for kanamycin can be achieved by naked eyes, with the visual limit of 35 nM. Meanwhile, a linear detection range of 1-30 nM with a low detection limit of 0.0778 nM for quantitative analysis can be achieved by using a scanning reader. The lateral flow strip biosensor exhibited high specificity and stability. Moreover, it was applied to detect kanamycin in various food samples, indicating its great potential in field testing.
A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for simultaneous determination of two hydrophilic aminoglycosides, kasugamycin and validamycin-A, in a variety of matrices (apples, cabbage, cucumbers, lettuce, tomatoes, and eggplant) has been developed. The proposed method provides sufficient sensitivity and excellent chromatographic performance using a special ReproSil 100 C18 column with 0.1% formic acid as the mobile phase additive. Accurate mass information for both analytes was obtained based on time-of-flight (TOF) mass spectrometry. The methanol/water (70-:-30, v/v) with pH adjusted to 5.5 was selected as the extraction solvent. The combination of hydrophilic-hydrophobic-balanced (HLB) cartridges with strong cation exchange SCX cartridges was used to purify the extracts with strongly polar compounds and satisfactory results were obtained. The consecutive solid-phase extraction minimized signal suppression/enhancement which led to matrix effects in the range of -12.6 to 6.11% only. Recovery experiments were performed for both compounds at three levels (50, 100, and 500 μg kg⁻¹) in six different matrices and yielded good recoveries ranging from 81.7% to 108% with relative standard deviation values below 13%. The limits of quantification (LOQs) for kasugamycin and validamycin-A were 4.1 μg kg⁻¹ and 1.0 μg kg⁻¹, respectively.
A simple and fast micellar liquid chromatographic (MLC) method for simultaneous analysis of the antibiotic fungicides of blasticidin S and kasugamycin was developed. Chromatographic separation was achieved on a Phenomenex® Aqua 5μ C 18 125 A column. The mobile phase consisted of an aqueous mixture of 69.3 mM sodium dodecyl sulfate (SDS) with deionized water (50 : 1, v/w). The flow rate was set at 1.0 mL/min, and the absorbance was monitored at 210 nm with a photodiode array detector. The total run time was less than 10 min, and the retention times (t r) were 2.47 min for blasticidin S ion, and 7.15 min for kasugamycin ion. Good linear relationships were obtained with correlation of coefficients (r) of 0.997 for kasugamycin, and 0.999 for blasticidin S. The limits of detection (LODs) of blasticidin S and kasugamycin were 0.5 μg/mL and 0.75 μg/mL, respectively, and the limits of quantitation (LOQs) for blasticidin S and kasugamycin were 1.5 μg/mL and 2.2 μg/mL, respectively. The recoveries of blasticidin S and kasugamycin in blank irrigation water ranged from 94.9-97.3% and 87.8-99.7%, respectively. By using MLC method blasticidin S and kasugamycin could be analyzed simultaneously.
