原位合成Bi3O4Br/Bi12O17Br2光催化剂及其对磺胺甲噁唑降解性能

Bi_xO_yBr_z光催化剂在有机药物废水处理领域有着非常广阔的潜在应用价值,但因光生电子和空穴的快速复合而表现出较低的光催化效率,进而限制了其应用范围。通过简易的水解-焙烧法原位制得一种新型的Bi₃O₄Br/Bi₁₂O₁₇Br₂复合光催化剂,并以磺胺甲噁唑(SMX)为模拟药物污染物进行了光催化性能测试,对所制催化剂进行了X射线衍射(XRD)、X射线光电子能谱(XPS)、扫描电子显微镜(SEM)、紫外可见漫反射光谱(UV-Vis DRS)、电化学阻抗(EIS)、光致发光光谱(PL)等表征。结果表明所制备的Bi₃O₄Br/Bi₁₂O₁₇Br₂复合光催化剂具有较强的光生载流子分离率、较低的界面电荷转移电阻,进而展示出优异的光催化降解SMX性能,在模拟太阳光下照射30 min,SMX降解率达到87%,相较于纯的Bi₃O₄Br和Bi₁₂O₁₇Br₂催化剂,降解率分别提升了30%和24%。最后基于自由基捕获实验和催化剂能带结构分析了所制催化剂的降解机理。     

A new ionic liquid surface‐imprinted polymer for selective solid‐phase‐extraction and determination of sulfonamides in environmental samples

Toward improving the selective adsorption performance of molecularly imprinted polymers in strong polar solvents, in this work, a new ionic liquid functional monomer, 1‐butyl‐3‐vinylimidazolium bromide, was used to synthesize sulfamethoxazole imprinted polymer in methanol. The resulting molecularly imprinted polymer was characterized by Fourier transform infrared spectra and scanning electron microscopy, and the rebinding mechanism of the molecularly imprinted polymer for sulfonamides was studied. A static equilibrium experiment revealed that the as‐obtained molecularly imprinted polymer had higher molecular recognition for sulfonamides (e.g., sulfamethoxazole, sulfamonomethoxine, and sulfadiazine) in methanol; however, its adsorption of interferent (e.g., diphenylamine, metronidazole, 2,4‐dichlorophenol, and m‐dihydroxybenzene) was quite low. ¹H NMR spectroscopy indicated that the excellent recognition performance of the imprinted polymer was based primarily on hydrogen bond, electrostatic and π‐π interactions. Furthermore, the molecularly imprinted polymer can be employed as a solid phase extraction sorbent to effectively extract sulfamethoxazole from a mixed solution. Combined with high‐performance liquid chromatography analysis, a valid molecularly imprinted polymer‐solid phase extraction protocol was established for extraction and detection of trace sulfamethoxazole in spiked soil and sediment samples, and with a recovery that ranged from 93–107%, and a relative standard deviation of lower than 9.7%.     

An overview of analytical methodologies for the determination of antibiotics in environmental waters

The widespread occurrence of antibiotics as contaminants in the aquatic environment has increased attention in the last years. The concern over the release of antibiotics into the environment is related primarily to the potential for the development of antimicrobial resistance among microorganisms. This article presents an overview of analytical methodologies for the determination of quinolone (Qs) and fluoroquinolone (FQs), macrolide (MLs), tetracycline (TCs), sulfonamide (SAs) antibiotics and trimethoprim (TMP) in different environmental waters. The analysis of these antibiotics has usually been carried out by high-performance liquid chromatography (HPLC) coupled to mass spectrometry (MS) or tandem mass spectrometry (MS/MS) and to a lesser extent by ultraviolet (UV) or fluorescence detection (FD). A very important step before LC analysis is sample preparation and extraction leading to elimination of interferences and prevention of matrix effect and preconcentration of target analytes.     

Simultaneous determination of sulfamethoxazole and trimethoprim in human plasma by capillary zone electrophoresis

A capillary electrophoretic method for the simultaneous determination of sulfamethoxazole and trimethoprim in plasma was developed. Sulfamethoxazole and trimethoprim extracted from human plasma with ethyl acetate were analyzed at 20 kV and 25 degrees C using 15 mm phosphate buffer (pH 6.2) as the electrolyte. The detection was by UV at 220 nm. The run time was 8.0 min and the limit of quantification was 10.00 microg/mL for sulfamethoxazole and 2.00 microg/mL for trimethoprim. The recovery was >99% for both compounds. This method enabled the detection of sulfamethoxazole and trimethoprim in plasma of patients after oral ingestion of their combined formulation. The present simple and rapid method is applicable to drug monitoring in immunocompromised patients who are taking the combined formulation of these compounds for the treatment or prophylaxis of Pneumocystis carinii pneumonia.     

磺胺甲恶唑在二硫化钼纳米片修饰电极上的电化学行为

采用了研磨后超声和离心分离方法制备了二硫化钼纳米片,通过原子力显微镜(AFM)和扫描电子显微镜(SEM)对不同离心速度分离的二硫化钼纳米片进行了表征。使用循环伏安法(CV)和差分脉冲伏安法(DPV)在磺胺甲恶唑溶液中对二硫化钼纳米片修饰的玻碳电极进行了电化学行为研究。结果显示,磺胺甲恶唑在二硫化钼修饰电极的循环伏安图上有一对氧化还原峰。其峰电流值与扫描速度的平方根成正比,是扩散控制过程。DPV扫描结果显示,磺胺甲恶唑的峰电流与其浓度之间存在着明显的线性关系。研磨超声方法制备出的二硫化钼纳米片层材料在电极上能够加速电子的转移和传输,从而有效提高峰电流值,为进一步研制准确测定磺胺甲恶唑电化学传感器提供了一种可选择的材料和电化学分析方法。     

薄层色谱扫描法同时测定增效联磺片中三组分含量的研究

 提出了增效联磺片中磺胺甲基异唑（ＳＭＺ）、磺胺嘧啶（ＳＤ）及甲氧节胺嘧啶（ＴＭＰ）三组分薄层色谱同时测定的新方法。该法以水饱和的乙酸乙酯－氯仿（２：１）的混合溶剂为展开剂，在硅胶ＧＦ＿（２５４）板上将被测各组分分离后，直接进行薄层色谱扫描测定，操作简便、快速，灵敏度高，重现性好。     

可变误差多面体法同时测定复方新诺明中二组分的含量

以可变误差多面体法处理多波长吸光光度数据同时测定了复方新诺明制剂模样和五个批号实际样品中磺胺甲恶唑（ＳＭＺ）,甲氧苯氨嘧啶（ＴＭＰ）的含量,１１份模拟样中ＳＭＺ、ＴＭＰ的回收率分别为９９．８％和１００．３％,复方新诺明片和注射液的测定结果与药典方法一致。     

乘子法在多组分光度分析中的应用

报道了将乘子法用于样品中多组分的分光光度法同时测定;介绍了乘子法的原理和计算步骤。对复方新诺明模拟样中磺胺甲恶唑、甲氧苄氨嘧啶测定的平均回收率分别为９９．７９％,１００．６７％,ＲＳＤ分别为０．４５％．０．９５％（ｎ＝９）,测定了５个批号复方新诺明片剂和针剂的含量,结果满意。     

4-(3-(4-羟基苯基) -3-氧代-1-芳基丙氨基)-N-(5-甲基异噁唑-3-基)苯磺酰胺的合成与抗糖尿病活性

由磺胺甲噁唑、对羟基苯乙酮和芳香醛反应直接合成了13个未见报道的β-氨基酮,反应选择性发生在羰基α位。产物结构通过¹H NMR、¹³C NMR、MS进行了表征。生物活性试验显示,低浓度范围,所得化合物不仅显示一定的蛋白质酪氨酸磷酸酶1B(PTP1B)和α-葡萄糖苷酶抑制活性,而且具有中等强度的过氧化物酶体增殖物激活受体反应元件(PPRE)的激动活性,8个化合物的激动活性超过40％,其中化合物11的活性达到72.7％。     

非线性偏最小二乘导数分光光度法同时测定复方新诺明中二组分的含量

构造了导数光谱与多组分浓度间的非线性模型 ,以偏最小二乘法估计模型参数 ,建立了同时测定两组分的非线性偏最小二乘导数分光光度法 ,方法用于复方新诺明中磺胺甲唑SMZ(Sulfamethoxazole)和甲氧苄啶TMP(Trimethoprim)含量的测定 ,10份模拟样中SMZ ,TMP的回收率分别为 99 8%和 10 0 1% ,RSD分别为 1 3%和 1 6 %。结果明显好于线性偏最小二乘导数分光光度法。用该法测定复方新诺明片中的二组分含量测定结果与药典方法一致 ,该法为复方制剂的分光光度分析提供了更为理想的新途径。