Gold immunochromatographic sensor for the rapid detection of twenty-six sulfonamides in foods

A gold immunochromatographic sensor (GICS) was developed for the rapid detection of 26 sulfonamides in honey samples.The sensor was based on a group-specific monoclonal antibody (mAb) that can recognize all 26 sulfonamides.Three haptens (hapten 1 with a thiazole ring,hapten 2 with a benzene ring,and hapten 3 with a straight carbon chain) were used for antigen preparation.With hybridoma technology,a group-specific mAb was screened with a 50％ maximal inhibitory concentration (IC50) against sulfathizole (STZ) and the other 25 analogues ranging from 0.08 to 90.18 ng/mL.Mono-dispersed gold nanoparticles were conjugated with the mAb to develop the lateral immunochromatographic strip.A labeled antibody concentration of 0.1 μg/mL and a coating antigen concentration of 0.2 μg/mL in the test line were chosen for strip preparation.Under optimized conditions,the visual limits of detection (vLOD) for the concentrations of STZ,sulfamethoxazole,sulfamethizole,sulfadiazine,sulfamerazine,sulfadimethoxine,sulfamonomethoxine,sulfameter,sulfamethoxypyridazine,and sulfachloropyridazine were 5,0.25,0.25,10,5,10,25,2.5,5,0.25,and 10 μg/kg,respectively.Scanner analysis in honey samples revealed good performance for detection of the 26 sulfonamides.Commercial honey samples were tested with the sensor and positive results were confirmed with high-performance liquid chromatography.The proposed strip sensor provides a convenient method for the rapid and reliable determination of sulfonamides pollutants in honey samples.     

肉制品中磺胺类药物的分子印迹聚合物的模拟研究

以磺胺类药物(SFAs)为模板分子,甲基丙烯酸(MAA)为功能单体,模拟研究磺胺类药物的分子印迹聚合物。通过密度泛函理论的计算,分析反应介质对印迹聚合物制备过程的影响,并从分子水平上研究SFAs-MAA之间的结合作用,为制备合理的印迹聚合物提供参考。     

UV-C辐照降解水中磺胺类药物

采用C类紫外线或称为短波紫外线（即UV-C）辐照降解水中磺胺类药物,考察了磺胺类药物种类、UV光强、磺胺类药物初始浓度、反应液pH对降解效果的影响。结果表明UV-C辐照对磺胺嘧啶、磺胺甲基嘧啶和磺胺甲恶唑的降解过程均符合拟一级反应动力学。UV-C辐照技术对磺胺甲恶唑的去除率最高,在反应液pH为7,光强为142μW/cm^2,初始浓度为0.02mmol/L条件下,辐照30 min后磺胺甲恶唑去除率达到67.80%,而磺胺嘧啶和磺胺甲基嘧啶去除率仅15%左右。通过增大紫外光强和减小初始浓度,可提高反应速率和磺胺甲恶唑去除率。反应液pH对反应效果的影响显著,酸性条件更利于UV-C辐照降解磺胺甲恶唑。     

微流控芯片联用高效液相色谱-荧光检测器同时测定肉类食品中4种磺胺类药物残留

摘 要：目的 建立一种使用微流控芯片进行肉类食品前处理以及结合高效液相色谱-荧光检测器(high performance liquid chromatography-fluorescence detector, HPLC-FLD)同时测定4种磺胺残留的方法。方法 样品先用乙酸乙酯提取,然后在微流控芯片中用2 mol/L盐酸溶液反萃取,同时正己烷脱脂,收集盐酸流出液100 μL,与0.5 g/mL醋酸钠溶液1：1混合,再加入0.2 g/L荧光胺50 μL,衍生化反应静置60 min后采用岛津ODS-3色谱柱进行分离,流动相为乙腈-2%乙酸水。结果 4种磺胺完全分离且在0.01~1 mg/L呈线性关系,在3个添加水平范围内,平均回收率为72.1%~91.6%,相对标准偏差为4.7%~13.6%,方法检出限为1~5 μg/kg。结论 该方法具有快速、方便、经济、除脂效果好、环保等优点,适合肉类食品中4种磺胺类药物残留分析,并且提供了一个新的样品前处理思路。     

Design,Synthesis, and in vitro Evaluation of Tubulin-Targeting Dibenzothiazines with Antiproliferative Activity as a Novel Heterocycle Building Block

We prepared a series of free NH and N-substituted dibenzonthiazines with potential anti-tumor activity from N-aryl-benzenesulfonamides. A biological test of synthesized compounds (59 samples) was performed in vitro measuring their antiproliferative activity against a panel of six human solid tumor cell lines and its tubulin inhibitory activity. We identified 6-(phenylsulfonyl)-6H-dibenzo[c,e][1,2]thiazine 5,5-dioxide and 6-tosyl-6H-dibenzo[c,e][1,2]thiazine 5,5-dioxide as the best compounds with promising values of activity (overall range of 2–5.4 μM). Herein, we report the dibenzothiazine core as a novel building block with antiproliferative activity, targeting tubulin dynamics.     

液相色谱-串联质谱法检测蜂蜜中15种喹诺酮类和17种磺胺类药物残留

目的建立同时测定蜂蜜中15种喹诺酮和17种磺胺类药物残留的液相色谱-串联质谱(liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)检测方法。方法样品经过磷酸盐缓冲溶液(pH=8)提取,过HLB(hydrophile-lipophile balance)固相萃取柱净化。以CORTECS C18色谱柱(2.1 mm×100 mm,1.6μm)分离,以5 mmol乙酸铵、0.1%甲酸水(A)和0.1%甲酸-乙腈(B)作为流动相进行梯度洗脱。质谱分析以电喷雾为离子源(electrospray ionization,ESI+),采用多反应监测(multiple reaction monitoring,MRM)。结果本方法在15 min内完成32种目标化合物的分离。15种喹诺酮和17种磺胺类药物在1.0、5.0和10.0μg/kg添加水平的回收率为54.9%~122.5%,相对标准偏差(relative standard deviation,RSD)小于18.7%(n=6),方法检出限为0.4μg/kg,定量限为1.0μg/kg。结论该方法快速、准确、灵敏,适合测定蜂蜜中喹诺酮和磺胺类药物残留。     

Development of a chemiluminescent enzyme‐linked immunosorbent assay for five sulfonamide residues in chicken muscle and pig muscle

BACKGROUND: An enzyme‐linked immunosorbent assay (ELISA) based on polyclonal antibodies with enhanced chemiluminescent (ECL) detection of sulfonamides in food samples has been optimised and characterised. The specificity of the assay was assessed by determining cross‐reactivities with a set of 16 sulfonamides. The aim of this study was to develop a method for determining sulfonamides with high sensitivity. RESULTS: The sensitivity of the developed ECL‐ELISA was higher than that of colorimetric ELISA. The sensitivities of five of the sulfonamides (sulfisozole, sulfathiazole, sulfameter, sulfamethoxypyridazine and sulfapyridine) ranged from 0.73 to 2.92 µg L^?1, with limits of detection of 0.10–0.43 µg L^?1. The coefficients of variation of intra‐assay and inter‐assay studies carried out over 5 days were mostly less than 10%. Recovery studies of chicken muscle and pig muscle were performed with simple and rapid extraction. Good recoveries (62.1–110.3%) were achieved and the results correlated well with those obtained using high‐performance liquid chromatography analysis. CONCLUSION: This study has provided an effective analytical technique for the rapid and reliable determination of residues of sulfisozole, sulfathiazole, sulfameter, sulfamethoxypyridazine and sulfapyridine in food samples with high sensitivity. To the authors' knowledge, this is the first report on chemiluminescent ELISA for sulfonamide analysis. Copyright © 2008 Society of Chemical Industry     

A New Mechanism of the Selective Photodegradation of Antibiotics in the Catalytic System Containing TiO2 and the Inorganic Cations

The mechanism of sulfisoxazole (SFF) selective removal by photocatalysis in the presence of titanium (IV) oxide (TiO₂) and iron (III) chloride (FeCl₃) was explained and the kinetics and degradation pathways of SFF and other antibiotics were compared. The effects of selected inorganic ions, oxygen conditions, pH, sorption processes and formation of coordination compounds on the photocatalytic process in the presence of TiO₂ were also determined. The Fe³⁺ compounds added to the irradiated sulfonamide (SN) solution underwent surface sorption on TiO₂ particles and act as acceptors of excited electrons. Most likely, the SFF degradation is also intensified by organic radicals or cation organic radicals. These radicals can be initially generated by reaction with electron holes, hydroxyl radicals and as a result of electron transfer mediated by iron ions and then participate in propagation processes. The high sensitivity of SFF to decomposition caused by organic radicals is associated with the steric effect and the high bond polarity of the amide substituent.     

Betulin Sulfonamides as Carbonic Anhydrase Inhibitors and Anticancer Agents in Breast Cancer Cells

Hypoxia-regulated protein carbonic anhydrase IX (CA IX) is up-regulated in different tumor entities and correlated with poor prognosis in breast cancer patients. Due to the radio- and chemotherapy resistance of solid hypoxic tumors, derivatives of betulinic acid (BA), a natural compound with anticancer properties, seem to be promising to benefit these cancer patients. We synthesized new betulin sulfonamides and determined their cytotoxicity in different breast cancer cell lines. Additionally, we investigated their effects on clonogenic survival, cell death, extracellular pH, HIF-1α, CA IX and CA XII protein levels and radiosensitivity. Our study revealed that cytotoxicity increased after treatment with the betulin sulfonamides compared to BA or their precursors, especially in triple-negative breast cancer (TNBC) cells. CA IX activity as well as CA IX and CA XII protein levels were reduced by the betulin sulfonamides. We observed elevated inhibitory efficiency against protumorigenic processes such as proliferation and clonogenic survival and the promotion of cell death and radiosensitivity compared to the precursor derivatives. In particular, TNBC cells showed benefit from the addition of sulfonamides onto BA and revealed that betulin sulfonamides are promising compounds to treat more aggressive breast cancers, or are at the same level against less aggressive breast cancer cells.