Spielmeyer Astrid, Ahlborn Jenny, Hamscher Gerd
Institute for Food Chemistry and Food Biotechnology, Justus Liebig University, Heinrich-Buff-Ring 58, 35392, Giessen, Germany,
Anal Bioanal Chem. 2014 Apr;406(11):2513-24. doi: 10.1007/s00216-014-7649-3. Epub 2014 Feb 18.
A new method for the analysis of sulfonamides and tetracyclines in heterogenic biogas plant input samples and fermentation residues is introduced. Veterinary antibiotics are only partially absorbed in the animal gut; therefore, animal manure can contain high loads of these substances. Animal manure is used for biogas generation, so antibiotics can enter the anaerobic fermentation process this way. However, only little is known about the fate of antibiotics within this process, also due to the lack of suitable analytical methods for this complex sample matrix. Therefore, we developed a method for the analysis of ten sulfonamides (sulfachloropyridazine, sulfadiazine, sulfadimethoxine, sulfaguanidine, sulfamerazine, sulfamethazine, sulfamethoxazol, sulfamethoxypyridazin, sulfapyridine, sulfathiazole) and four tetracyclines (chlortetracycline, doxycycline, oxytetracycline, tetracycline) in biogas plant input and output samples, including a single liquid-liquid-extraction step and analysis via liquid chromatography (LC) and triple quadrupole mass spectrometry. The detection limit of this method ranges from 0.01 to 0.08 mg kg(-1). Matrix calibration using antibiotic-free cattle feces and isotopic-labeled internal standards enables quantification of antibiotics in different matrices such as animal manure, dung, or fermenter outputs with recovery rates between 70 and 130 %. This makes the method suitable for investigating the fate of antibiotics in animal manure and fermentation processes. A screening of 15 German biogas plants revealed the presence of several antibiotics up to 9 mg kg(-1) (201 mg kg(-1) dry matter). During the fermentation process, elimination occurs; however, with the exception of chlortetracycline, the antibiotic content remains in the same order of magnitude.
介绍了一种分析异质沼气厂输入样品和发酵残留物中磺胺类药物和四环素类药物的新方法。兽用抗生素在动物肠道中仅部分被吸收；因此，动物粪便中可能含有大量此类物质。动物粪便被用于沼气生产，因此抗生素可通过这种方式进入厌氧发酵过程。然而，由于缺乏适用于这种复杂样品基质的分析方法，人们对该过程中抗生素的去向了解甚少。因此，我们开发了一种分析沼气厂输入和输出样品中十种磺胺类药物（磺胺氯哒嗪、磺胺嘧啶、磺胺二甲氧嘧啶、磺胺脒、磺胺甲基嘧啶、磺胺二甲嘧啶、磺胺甲恶唑、磺胺甲氧嗪、磺胺吡啶、磺胺噻唑）和四种四环素类药物（金霉素、强力霉素、土霉素、四环素）的方法，包括一步液液萃取步骤，并通过液相色谱（LC）和三重四极杆质谱进行分析。该方法的检测限为0.01至0.08 mg kg⁻¹。使用不含抗生素的牛粪和同位素标记内标进行基质校准，能够对不同基质（如动物粪便、粪肥或发酵罐输出物）中的抗生素进行定量，回收率在70%至130%之间。这使得该方法适用于研究动物粪便和发酵过程中抗生素的去向。对15家德国沼气厂的筛查发现，存在几种含量高达9 mg kg⁻¹（干物质含量为201 mg kg⁻¹）的抗生素。在发酵过程中，抗生素会被去除；然而，除金霉素外，抗生素含量仍保持在相同数量级。
