磺胺二甲嘧啶分子印迹聚合物的合成及其识别性能

磺胺二甲嘧啶分子印迹聚合物的合成及其识别性能;磺胺二甲嘧啶;分子印迹聚合物;硅胶;分子识别     

Optimization of sulfamethazine sodium adsorption onto activated carbon-based Salix psammophila: investigation of adsorption behavior and mechanism

A study on the adsorption of sulfamethazine sodium (SMS) from aqueous solution onto the activated carbon (AC)-based Salix psammophila (SP) by phosphoric acid activation was conducted. The central composite design under response surface methodology was employed for the removal of SMS and the process parameters were optimized. Influence of adsorbent dose, initial concentration of SMS, contact time and solution pH on the adsorption capacity of AC was investigated. The optimum adsorption conditions were obtained using adsorbent dosage of 0.54?g/L, initial concentration of 322?mg/L, contact time of 8?hours, pH value of 4.04. Kinetic studies showed the adsorption followed a pseudo-second-order model and Elovich model. The experimental equilibrium data were fitted Koble-Corrigan model and Freundlich model well and the maximum monolayer adsorption capacity of AC calculated by Langmuir model was 338.58?mg/g at 25?°C. In addition, AC was characterized by the SEM–EDS, BET, FITR and point of zero charge (pH_pzc). The mechanisms of SMS sorption onto AC were explored. Desorption and regeneration tests were carried out to evaluate the feasibility of reusing the AC. This study indicated the AC prepared from SP was an excellent adsorbent with the low cost and high performance.     

An appropriate and systematized procedure for validating qualitative methods: Its application in the detection of sulfonamide residues in raw milk

The lack of well-established references for the validation of qualitative analyses and the increasing demand for reliable binary responses were the main motivating factors for this study. A detailed procedure for single-laboratory validation of qualitative methods is proposed. The experimental design and the tools for data analysis were based on the theoretical background, as well as the aspects of efficiency, convenience and simplicity. Four experimental steps were defined, as follows: (i) preliminary tests for the determination of the concentration range, (ii) a study of the rates, unreliability region, detection limit, and the accordance and concordance values, (iii) a study of the selectivity in the presence of known interferences, and (iv) a study of robustness. The applicability of the procedure was demonstrated by the validation of a qualitative commercial kit for detecting sulfonamide residues in raw milk using both the visual and instrumental reading techniques. Reliability rates of 100% were obtained for the blank samples. For the samples spiked with sulfamethazine at 10.8 and 108 μg L⁻¹ and with sulfadimethoxine or sulfathiazole at 10 and 100 μg L⁻¹, the reliability rates ranged from 93.3 to 100%. Selectivity was demonstrated using trimethoprim as a potential interferent. The method was considered robust for the factors of the temperature (54 and 58 °C) and time (6 and 10 min) for incubating the test strips. The estimated detection limits and unreliability regions confirmed the suitability of the kit for this purpose, based on the legislated residue limits.     

Pyridine and 3‐methylpyridine solvates of the triple sulfa drug constitutent sulfamethazine

Sulfonamides display a wide variety of pharmacological activities. Sulfamethazine [abbreviated as SMZ; systematic name 4‐amino‐N‐(4,6‐dimethylpyrimidin‐2‐yl)benzenesulfonamide], one of the constitutents of the triple sulfa drugs, has wide clinical use. Pharmaceutical solvates are crystalline solids of active pharmaceutical ingredients (APIs) incorporating one or more solvent molecules in the crystal lattice, and these have received special attention, as the solvent molecule can impart characteristic physicochemical properties to APIs and solvates, therefore playing a significant role in drug development. The ability of SMZ to form solvates has been investigated. Both pyridine and 3‐methylpyridine form solvates with SMZ in 1:1 molar ratios. The pyridine monosolvate, C₁₂H₁₄N₄O₂S·C₅H₅N, crystallizes in the orthorhombic space group Pna 2₁, with Z = 8 and two molecules per assymetric unit, whereas the 3‐methylpyridine monosolvate, C₁₂H₁₄N₄O₂S·C₆H₇N, crystallizes in the orthorhombic space group P 2₁2₁2₁, with Z = 4. Crystal structure analysis reveals intramolecular N—H…N hydrogen bonds between the molecules of SMZ and the pyridine solvent molecules. The solvent molecules in both structures play an active part in strong intermolecular interactions, thereby contributing significantly to the stability of both structures. Three‐dimensional hydrogen‐bonding networks exist in both structures involving at least one sulfonyl O atom and the amine N atom. In the pyridine solvate, there is a short π–π interaction [centroid–centroid distance = 3.926 (3) Å] involving the centroids of the pyridine rings of two solvent molecules and a weak intermolecular C—H…π interaction also contributes to the stability of the crystal packing.     

Sulfamethazine and Sulfadimethoxine Separation Strategies Based on Molecularly Imprinted Adsorbents

Abstract

The synthesis of molecularly imprinted polymer (MIP) as a stationary phase of high‐performance liquid chromatography (HPLC), for the efficient determination of sulfamethazine and sulfadimethoxine in tablets is reported. The polymers were prepared by a noncovalent method with sulfamethazine as the template, methacrylic acid as the functional monomer and ethylene glycoldimethacrylate as the cross‐linker in the presence of chloroform as the solvent. The retention time of sulfamethazine and sulfadimethoxine were approximately 5.2±0.2 and 10.3±0.5 min, respectively. In order to compare the chromatographic data from the stationary phase, retention factor (k) and separation factors (α) were given. The values of α were 2.05～2.17 showed that the MIP was able to recognize structurally subtle differences from the template molecule.

The MIP was successfully applied to commercial tablet analysis and the result showed a good recovery with 99 and 98% for sulfamethazine and sulfadimethoxine.     

Imaging Array SPR Biosensor Immunoassays for Sulfamethoxazole and Sulfamethazine

A homemade array surface plasmon resonance (SPR)-based imaging biosensor was used to develop sensitive and fast immunoassays to determine sulfamethoxazole (SMOZ) and sulfamethazine (SMT) in buffer. Two conjugations of sulfonamide-bovine serum albumin (BSA) were separately immobilized on two different rows of the array chip with one row as reference. The immobilization was carried out in the instrument to monitor the quantity of the conjugations immobilized. The antibody mixed with the sulfonamide in the buffer was injected over the surface of the chip to get a relative response which was inversely proportional to the concentration of the sulfonamide in the PBS buffer. Two calibration curves were constructed and the limit of detection for sufamethoxazole in buffer was 3.5 ng/mL and for sulfamethazine 0.6 ng/mL. The stability and specificity of the antibody were also studied. The monoclonal antibody did not bind with BSA.