排序方式: 共有61条查询结果,搜索用时 15 毫秒
1.
Ai Jia Yang Xiao Jianying Hu Mari Asami Shoichi Kunikane 《Journal of chromatography. A》2009,1216(22):4655-4662
A sensitive method was developed for the trace determination of six tetracyclines and ten of their degradation products in influent, effluent, and river waters using liquid chromatography–electrospray tandem mass spectrometry detection, combined with Oasis hydrophilic–lipophilic balance (HLB) cartridge extraction and Oasis mixed-mode strong anion exchange (MAX) cartridge cleanup. Tetracyclines and their products were separated by liquid chromatography in 9.5 min, and the instrument detection limits were generally between 0.03 and 0.1 μg/L except for minocycline (0.5 μg/L). The chromatograms were improved through the MAX cleanup and no apparent matrix effect was found. The recoveries of all the target compounds except for 4-epianhydrochlortetracycline and anhydrochlortetracycline (34–52%) were 75–120% for influent, 61–103% for effluent, and 64–113% for river waters. The method detection limits (MDLs) of the analytes varied in the range of 0.8–17.5 ng/L in all studied matrices. The method was applied for the determination of tetracyclines and their products in a sewage treatment plant (STP) and surface waters in Beijing, China. Oxytetracycline (3.8–72.5 ng/L), tetracycline (1.9–16.5 ng/L), and five products including 4-epitetracycline, 4-epioxytetracycline, isochlortetracycline, anhydrotetracycline, and 4-epianhydrochlortetracycline (5.7–25.3 ng/L) were detected in wastewater, while only oxytetracycline and tetracycline (2.2 and 2.1 ng/L) were detected in surface water samples. 相似文献
2.
Merike Lillenberg Sergei Yurchenko Karin Kipper Koit Herodes Viljar Pihl Kalev Sepp Rünno Lõhmus Lembit Nei 《Journal of chromatography. A》2009,1216(32):5949-5954
A new scheme for the quantitative determination of traces of fluoroquinolones (FQs), tetracyclines (TCs) and sulfonamides (SAs) in sewage sludge was developed. The compounds were simultaneously extracted from sewage sludge by pressurized liquid extraction (PLE). A novel and effective method for PLE was developed. Solid-phase extraction was used for cleaning up the extracts. Identification and quantification of the compounds was done using high-performance liquid chromatography with electrospray ionization mass spectrometry in selected reaction monitoring mode. The best recovery of FQs and TCs was obtained by using hydrophilic–lipophilic balance cartridges, recoveries ranged 59% for norfloxacin to 82% for ofloxacin and 95% for doxycycline; for SAs strong cation-exchange cartridges were more efficient, recoveries were 96% for sulfamethoxazole and 43% for sulfadimethoxine. Limit of quantification ranged from 0.1 ng/g for SAs to 160 ng/g for tetracycline. Method precision for TCs was 5.06% and 1.12%, and for SAs 0.43% and 2.01%. FQs precision ranged from 0.77% to 1.89%. 相似文献
3.
4.
An important step in the validation of an analytical procedure is the study of its robustness. In the case of spectrofluorimetric determinations, quenching introduces specific problems which are approached in this paper for the particular case of tetracyclines determination in milk. Quenching can be detected with excitation emission matrices (EEM) signals and a three-way Parallel Factor (PARAFAC) decomposition and modelled by means of a four-way PARAFAC decomposition which reproduces the physical model of this effect.The robustness of the method is evaluated by including changes in seven experimental variables: trichloroacetic acid (TCA) volume solution used in the precipitation of milk proteins, revolutions per minute, time and temperature in the centrifugation step, pH and emission-excitation slit width in the fluorimetric analyte determination and the analyst. The robustness analysis is carried out by means of a Plackett-Burman experimental design as it is suggested by European Decision 2002/657/EC (European Decision (EC) No. 2002/657/EC of 12 August 2002, implementing Council Directive 96/23/EC, concerning the performance of analytical methods and the interpretation of results, Off. J.L 221, 17/8/2002, 8). The analyte concentration will be taken as response in the Plackett-Burman experimental design instead of the signal as it is habitual in these cases. Therefore, a three-way Partial Least Squares (3-PLS) calibration models with EEM signal is needed.When an analogous study is carried out for tetracycline (TC) in the absence of chlorotetracycline (CTC) as interferent, univariate calibration is employed, being able to conclude that in the robustness analysis, different factors are significantly active when quenching exists. 相似文献
5.
Determination of oxytetracycline and some impurities in plasma by non-aqueous capillary electrophoresis using solid-phase extraction 总被引:1,自引:0,他引:1
Summary The potential of a non-aqueous, capillary electrophoresis (NACE) system for separating oxytetracycline from three of its impurities—tetracycline,
4-epioxytetracycline and 4-epitetracycline—using UV detection has been studied. The running buffer was: 25 mM sodium acetate,
1 mM EDTA, methanesulfonic acid, pH 4, dissolved in MeOH-ACN (50∶50,v/v). The method was also used to determine these compounds in pig plasma. A solid-phase extraction (SPE) procedure as a clean-up
step has also developed. For this we tested Sep Pak C18, LiChrolut EN and OASIS cartridges. OASIS cartridges were best. Recoveries were 90–100% for all compounds except EOTC which
had a recovery of 74%. 相似文献
6.
A novel application of an electrochemical biosensor is here employed as analytical method for the detection and presumptive identification of antimicrobial drug residues in milk. The measurement was based on carbon dioxide production rate in relation to inhibition of microbial grow (Escherichia coli ATCC 11303). In this pilot study quinolone and tetracycline residues have been taken into consideration because use of these last in livestock production has been identified as area of particular concern. The experimental approach and analytical method developed appear adequate for the purpose, and compared to older screening methods as, for example, the microbial inhibition assays and immunoassays, offers the advantages of (i) very short analysis time (about 120 min); (ii) smaller sample amount (approximately 0.5 mL); (iii) no sample treatment (iv) good precision; and (v) the possibility of following, in a continuous manner, the inhibition process. Moreover, sensitivity of electrochemical biosensor system is resulted very high considering that for all quinolones and tetracyclines investigated it has been possible detect a residue concentration below or equal to 25 μg L−1. Under this point of view, it must be considered that the maximum residue limits fixed by UE for quinolones and tetracyclines in milk are, at present, all higher of this concentration. 相似文献
7.
Determination of tetracyclines residues in honey by on-line solid-phase extraction high-performance liquid chromatography 总被引:3,自引:0,他引:3
An automated system using on-line solid-phase extraction (SPE) high-performance liquid chromatography (HPLC) with ultraviolet (UV) detection was developed for the determination of tetracyclines (TCs), such as tetracycline (TC), oxytetracycline (OTC), chlortetracycline (CTC), metacycline (MC), and doxycycline (DC) in honey. One milliliter diluted honey sample was injected into a conditioned C18 SPE column and the matrix was washed out with water for 3 min. By rotation of the switching valve, TCs were eluted and transferred to the analytical column by the chromatographic mobile phase. Chromatographic conditions were optimized. TCs were separated in less than 8 min with a gradient elution using a mixture of 0.8% formic acid and acetonitrile. The UV detection was performed at 365 nm. The conditions for on-line SPE, including solvent and total time for loading sample and washing matrix were also optimized. Time for extraction and separation decreased greatly. For the five kinds of TCs, the limits of detection (LODs) at a signal-to-noise of 3 ranged from 5 to 12 ng g−1. The relative standard deviations (R.S.D.) for the determination of TCs ranged from 3.4 to 7.1% within a day and ranged from 3.2 to 8.9% in 3 days, respectively. 相似文献
8.
9.
Spisso BF de Oliveira e Jesus AL de Araújo MA Monteiro MA 《Analytica chimica acta》2007,581(1):108-117
A high-performance liquid chromatography-fluorescence detection method was optimized and validated to determine tetracyclines residues in bovine milk. Post-column derivatization using metal complexation in non-aqueous reagent increased the fluorescence of chelates by a factor up to 2.54 compared to water (signal-to-noise ratio enhancement). Overall recoveries ranged from 61 to 115%, with RSDr from 5 to 15% (n = 54). Detection limits ranged from 5 to 35 μg kg−1. Limits of quantification were established at 50 μg kg−1. Decision limits (CCα) were 109, 108 and 124 μg kg−1 and detection capabilities (CCβ) 119, 117 and 161 μg kg−1 for oxytetracycline, tetracycline and chlortetracycline, respectively. The method was applied successfully in a national monitoring program. 相似文献
10.
Treetepvijit S Preechaworapun A Praphairaksit N Chuanuwatanakul S Einaga Y Chailapakul O 《Talanta》2006,68(4):1329-1335
The electrochemical analysis of tetracyclines was investigated using nickel-implanted boron-doped diamond thin film electrode (Ni-DIA) by cyclic voltammetry and high performance liquid chromatographic with amperometry. Cyclic voltammetry was used to study the electrochemical oxidation of tetracyclines. Comparison experiments were carried out utilizing as-deposited BDD and glassy carbon electrodes. Ni-DIA electrode provided well-resolved oxidative irreversible cyclic voltammograms and the highest current signals among the electrode studied. High performance liquid chromatography (HPLC) with amperometric detection was also studied. The chromatography was performed using a commercially available Inertsil C18 column, with the mobile phase being: 80% phosphate buffer (pH 2.5)-20% acetonitrile and detected at 1.55 V. The methods were validated over the concentration range 0.05-100 ppm with the overall average recoveries from 83.3 to 102.5% and R.S.D. of less than 10%. The proposed method was further applied to analyse shrimp samples. 相似文献