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Simple Quantitation of Flucytosine in Low Volume serum samples and Evaluation of Common Endogenous Interferences by HPLC-UV

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American Journal of Analytical Chemistry 2022年第9期13卷 289-299页

作者： Abdul Rafiq Khan Ali Alothaim Waleed Tamimi Majid Alshaibani Souad Marwan Al Enazi Syed Muhammad Saad Khalid Mohammed Khan Department of Pathology and Laboratory Medicine King Abdulaziz Medical City Riyadh KSA Department of Chemistry University of Karachi Karachi Pakistan H. E. J. Research Institute of Chemistry International Center for Chemical and Biological Sciences University of Karachi Karachi Pakistan

5-Fluorocytosine (5-FC) is used for the treatment of several infections. It is extremely important to monitor blood level concentration for maximum activity to avoid its side effects. A simple, faster, and more accurate analytical method is developed and validated using high-performance liquid chromatography with UV detection in a very low-volume serum sample. Exactly 50 μL of serum was precipitated with 5% trichloroacetic acid. After mixing and centrifugation, 20 μL of supernatant was injected into the HPLC column. Detection was performed at 280 nm. The method is very specific and free from interfering substances due to different drugs and their different circulating metabolites. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.50 μg/L and 1.0 μg/L, respectively. The method was linear in the range of 5 - 150 μg/L in the serum sample. In method comparison, the correlation coefficient r2 was 0.999 and the percentage recovery was 90% - 105% on four levels of the quality control samples. Within run and between run precision was found to be less than 2.2% at four different concentrations (5, 25, 50, and 100 μg/L). A simple, faster, and more accurate HPLC-UV method is developed which is very useful for monitoring 5-FC concentration in low volume serum samples without evaporation step and ion exchange chromatography within minutes.

关键词： 5-Fluorocytosine serum sample HPLC-UV Method Quantification Validation

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A novel luminol-based chemiluminescence method for the determination of amikacin sulfate in serum by using trivalent copper-periodate complex

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Journal of Pharmaceutical Analysis 2013年第5期3卷 360-366页

作者： Yu-Fei Hu Gong-Ke Li Zhu-Jun Zhang School of Chemistry and Chemical Engineering Sun Yat-sen University Department of Chemistry Institute of Analytical Science Southwest University

A novel chemiluminescence （CL） reaction was based on the oxidizing reaction of luminol by the trivalent copper-periodate complex （Ks[Cu（HIO6）2], DPC） in alkaline medium. The CL intensity could be enhanced in the presence of amikacin sulfate （AKS）. A new CL method was developed for the determination of AKS by coupling with flow injection （FI） technology. Because of the distinctive oxidative effect of DPC, the luminol-based CL reaction could occur at a low concentration of 10-7 M. The relative CL intensity was proportional to the concentration of AKS in the range of 4.0 x 10-9-4.0 x 10-6 g/mL with the detection limit of 1.2 x 10-9 g/mL. The relative standard deviation was 2.1% for 8.0xl0-9g/mL AKS （n=9）. The proposed method was successfully applied to the direct determination of AKS at the level of ng/mL in serum samples. The recovery varied from 97.0% to 106.3%. A possible mechanism of the CL reaction was discussed in detail by relating to the CL kinetic characteristics and electrochemical activities of the oxidant DPC.

关键词： Amikacin sulfate Chemiluminescence K5 [Cu(HIO6)2 ] Flow injection serum sample

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Electrochemical Study on the Interaction of Protein with Bromothymol Blue and Its Analytical Application

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Chemical Research in Chinese Universities 2008年第6期24卷 701-706页

作者： WANG Xue-liang YANG Jie JIAO Kui College of Chemistry and Molecular Engineering Qingdao University of Science and Technology Qingdao 266042 P. R. China

The interaction of bromothymol blue（BB） with human serum albumin（HSA） was studied by electrochemical techniques and a sensitive method for proteins assay was developed. When BB interacted with HSA, the voltammetric peak current value of BB decreased linearly with the concentration of HSA in a range of 1.0--40.0 mg/L, and the peak potential shifted negatively. Based on the results, a sensitive assay method for proteins, such as HSA, bovine serum albumin（BSA）, and egg albumin etc. was established. This method was further applied to determining the HSA in healthy human blood samples, and the results are not significantly different from those obtained by the classic Coomassie Brilliant Blue G-250 spectrophotometic method. The detecting conditions of this method were optimized and the interaction mechanism was discussed. The results show that the electrochemical parameters（formal potential E^0, standard rate constant of the electrode reaction ks, parameter of kinetic nα） of BB have no obvious changes before and after the interaction, which indicate that BB can interact with HSA, forming an electrochemical non-active complex. The equilibrium constant（βs） and the binding ratio（m） for this complex were calculated. The m is 4 and βs is 1.41 × 10^19. This method is fast, simple, highly sensitive, and has good selectivity, which can be used in clinical measurements.

关键词： Bromothymol blue(BB) Human serum albumin serum sample Voltammetry

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Highly selective and sensitive “swatch–on” fluorescence sensor of ascribe acid based on the cysteamine-coated CdTe quantum dots and cerium(Ⅳ)

Highly selective and sensitive “swatch–on” fluorescence s...

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河南省化学会2016年学术年会

作者： Jingjing Du Ran Yang Haichen Mao Jianjun Li Lingbo Qu The College of Chemistry and Molecular Engineering Zhengzhou University

Cysteamine-coated Cd Te quantum dots(CA-CdTe QDs) was synthesized by a simple hydrothermal method employing cadmium chloride as cadmium source and cysteamine hydrochloride as functional monomer. The fluorescence of as-synthesized CA-Cd Te QDs was could be intensively quenched by cerium(Ⅳ)(Ce) though an photo-induced electron transfer(PET) to form a non-luminescent complexes of CA-Cd Te-Ce. When reductive ascorbic acid(AA) was introduced to CA-Cd Te-Ce, Ce was reduced to Ce, the fluorescence of CA-Cd Te QDs was restored. Based on such phenomena, a"switch-on" fluorescence approach for sensing of ascorbic acid(AA) was developed. Under the optimal conditions, the CA-Cd Te QDs showed high positive electricity and had obvious electrostatic repulsion to the positively charged reductive molecules such as uric acid, dopamine and glutathione, which make them not effectively reacting with Ce. Owing to such a special eletrostatic repulsion effect and the difference of reducing capacity, the proposed method showed excellent sensitivity and selectivity for AA detection in a wide linear relationship from 0.03-33.0 μM, the detection limit was as low as 11.0nM. This is very different from those for the traditional redox-based fluorescence probes. Furthermore,the as-fabricated fluorescent sensing system was successfully applied to the analysis of AA in human serum sample with satisfactory results. The work described in this paper provides new design strategy and valuable platform for highly selective AA sensing in clinic diagnostic and drug screen.

关键词： ascorbic acid cysteamine-coated CdTe quantum dots fluorescence switch-on serum sample

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