表面增强拉曼光谱与薄层色谱结合对磺胺类药物的研究

报告了应用表面增强技术将薄层色谱与ＦＴ－Ｒａｍａｎ光谱结合获得磺胺嘧啶和磺胺二甲基嘧啶光谱新方法的研究。研究表明，在薄层色谱原位３μｇ样品的ＦＴ－ＮＩＲ－ＳＥＲＳ谱与固体的Ｒａｍａｎ光谱基本一致，比银溶胶－分子体系有更好的表面增强效果，灵敏度高，并能可靠地反映分子的精细结构信息。     

Assessment of veterinary drugs present in pork kidney from a Midwest US retail market

A total of 1040 pork kidneys were purchased from 4 retail stores located in a Midwestern US town and screened for antibiotics with the Charm-KIS? screening test. Six samples (0.6%) tested positive with the Charm-KIS?. Sixty-five samples from each retail location and the 18 Charm-KIS? positive or ‘caution’ samples were also subjected to ELISA to determine the presence of commonly used veterinary drugs including flunixin, ractopamine, sulfamethazine, and/or tetracycline of the 278 samples assessed by ELISA, flunixin, ractopamine, sulfamethazine, and tetracycline residues were found to be 0%, 22%, 4%, and 10% ELISA positive respectively, and had greater than limit of quantitation concentrations as measured by LC-MS/MS. All residue levels determined by LC-MS/MS were well below US tolerances, regardless of analyte. These findings suggest that veterinary drugs are being used in accordance with US regulations and that veterinary drug residues in pork do not pose a health concern to US consumers.     

磺胺二甲嘧啶的示波极谱法分析

研究了磺胺二甲嘧啶（ＳＭ２）的示波极谱法。磺胺二甲嘧啶在０．０１ｍｏｌ／ＬＨＣｌ介质中于－０．９９５Ｖ附近出现一清晰的阴极还原波。在１×１０－７～１×１０－４ｍｏｌ／Ｌ范围内，浓度与波高有良好的线性关系。检测下限可达３．０×１０－９ｍｏｌ／Ｌ。测定了小儿胺散中的ＳＭ２的含量，与紫外－可见分光光度法对照，结果一致。测定了尿样中ＳＭ２的含量，结果令人满意。     

Novel approach to control sulfamethazine misuse in food-producing animals by hair analysis

The presence of sulfamethazine residues in pig and calf hair was compared with the residual levels encountered in the corresponding edible tissues (liver and muscle) as a consequence of drug administration. Sulfamethazine up to 84.7 mg kg^-1 was found in calf hair samples after a pharmacological treatment, with a significant effect of hair pigmentation. High concentrations of the parent drug were detected in calf hair for 4 weeks after administration, when sulfamethazine residues were no longer detectable in the corresponding edible tissues. In a similar way, pig hair also accumulated sulfamethazine residues up to 40.5 mg kg^-1, which was more than the amount detected in the corresponding muscle and liver samples at slaughter. Hair analysis seems a suitable tool to improve the efficacy of regulatory controls, and thus the safety of the food chain and to discourage the improper use of sulfamethazine in animal farming.     

Simultaneous detection of sulfamethazine and sulfaquinoxaline using a dual-label time-resolved fluorescence immunoassay

A dual-label time-resolved fluoroimmunoassay (TRFIA) was introduced for the simultaneous quantification of sulfamethazine (SM₂) and sulfaquinoxaline (SQX). Lanthanide (Eu³⁺ and Sm³⁺)-labelled antibodies were used because lanthanides have higher stabilities and narrower emission spectra than most fluorescent dyes. The sensitivity of the TRFIA for SM₂ was 0.02 ng ml^?1, and the average recoveries and the intra- and inter-assay CVs were 77.2–107.6%, 5.4–10.5%, and 6.0–11.2%, respectively. The sensitivity of the TRFIA for SQX was 0.04 ng ml^?1; and the average recoveries and the intra- and inter-assay CVs were 74.1–102.8%, 4.6–10.9%, and 8.7–11.2%, respectively. The method was used to analyse chicken tissue and egg samples, and the results agreed well with the results of HPLC and enzyme-linked immunosorbent assay (ELISA) analyses, with correlation coefficients (R²) of 0.9415–0.9724. The TRFIA developed is a simple, fast and sensitive method for the high-throughput simultaneous screening of SM₂ and SQX in edible animal tissues.     

Rapid and Sensitive Immunochromatographic Strip for On‐site Detection of Sulfamethazine in Meats and Eggs

A rapid immunochromatographic (ICG) strip based on a conjugate of colloidal gold and monoclonal antibody (mAb) was developed for the rapid, sensitive, and on‐site detection of sulfamethazine in meat and egg samples. The detection limit of the ICG strip is 2 ng/mL, and the assay can be completed in 10 min. A cross‐reactivity test indicated that the ICG strip was highly specific to sulfamethazine with no cross‐reaction with sulfonamide compounds and other antibiotics. The results of the recovery test from meat and egg samples spiked with sulfamethazine were in good agreement with those obtained by the indirect competitive enzyme‐linked immunosorbent assay. These results demonstrated that the ICG strip can be used as a rapid and qualitative tool for on‐site screening of sulfamethazine in meat and egg samples.     

SM_2人工抗原合成研究

采用重氮化法合成磺胺二甲嘧啶(SM2)-人血清白蛋白(HAS)免疫抗原和SM2-卵清白蛋白(OVA)包被抗原。经紫外光谱扫描法确认SM2与载体蛋白偶联成功;经计算得SM2与HSA、OVA的结合比分别为9:1和15:1。     

利用表面等离子谐振生物传感器检测磺胺二甲嘧啶的方法研究

动物源性食品中的兽药残留对人类的健康具有潜在的危害。这项研究利用SPR生物传感器免疫法检测磺胺二甲嘧啶。实验对抗原在芯片表面的固定条件以及抗体的浓度进行了优化,实验中所构建的标准曲线的检测限(LOD)约为0.7ng/ml,检测范围为0.7～10ng/ml。对抗体的特异性和稳定性进行了研究。SPR-2004传感器为中国科学院电子学研究所自行研制的生化分析仪,为单通道双参数型,可以通过使用参照表面来消除折射率和基质效应的影响,从而提高数据的准确性,并缩短检测时间。     

无标记免疫分析——表面等离子体共振检测方法研究

利用表面等离子体共振生物传感器对磺胺嘧啶及磺胺二甲嘧啶进行快速无标记检测研究,优化反应条件。抗原固定缓冲液pH为4.2~4.8;抗体浓度为1∶100～1∶200倍稀释;再生液为0.1mol/LH₃PO₄溶液,再生时间为1.5min。研究建立了标准曲线,并对芯片的稳定性进行了考察。