Haller Michel Y, Müller Stephan R, McArdell Christa S, Alder Alfredo C, Suter Marc J F
Swiss Federal Institute for Environmental Science and Technology (EAWAG), Dübendorf.
J Chromatogr A. 2002 Apr 5;952(1-2):111-20. doi: 10.1016/s0021-9673(02)00083-3.
A fast and cost effective method was developed to extract and quantify residues of veterinary antimicrobial agents (antibiotics) in animal manure by liquid-liquid extraction and liquid chromatography-mass spectrometry. The compounds investigated include six sulfonamides, one metabolite, and trimethoprim. The method was performed without sample clean up. Recoveries from spiked manure slurry samples (spike level = 1 mg/kg) were as follows: sulfaguanidine (52%), sulfadiazine (47%), sulfathiazole (64%), sulfamethazine (89%), its metabolite N4-acetyl-sulfamethazine (88%), sulfamethoxazole (84%), sulfadimethoxine (51%), and trimethoprim (64%). Relative standard deviations of the recoveries were less than 5% within the same day and less than 20% between days. The limit of quantification was below 0.1 mg/kg liquid manure slurry for all compounds and calibration curves obtained from extracts of spiked samples were linear up to a level of 5 mg/kg liquid manure, except for trimethoprim (0.01-0.5 mg/kg). Analysis of six grab samples taken in Switzerland from manure pits on farms where medicinal feed had been applied revealed total sulfonamide concentrations of up to 20 mg/kg liquid manure.
开发了一种快速且经济高效的方法，通过液液萃取和液相色谱 - 质谱法来提取和定量动物粪便中兽用抗菌剂（抗生素）的残留量。所研究的化合物包括六种磺胺类药物、一种代谢物和甲氧苄啶。该方法无需进行样品净化。加标粪便泥浆样品（加标水平 = 1 mg/kg）的回收率如下：磺胺胍（52%）、磺胺嘧啶（47%）、磺胺噻唑（64%）、磺胺二甲嘧啶（89%）、其代谢物N4 - 乙酰磺胺二甲嘧啶（88%）、磺胺甲恶唑（84%）、磺胺二甲氧嘧啶（51%）和甲氧苄啶（64%）。回收率的相对标准偏差在同一天内小于5%，不同天之间小于20%。所有化合物的定量限均低于0.1 mg/kg液体粪便泥浆，并且从加标样品提取物获得的校准曲线在液体粪便水平高达5 mg/kg时呈线性，甲氧苄啶除外（0.01 - 0.5 mg/kg）。对瑞士从使用过药物饲料的农场粪坑采集的六个抓取样品进行分析，结果显示液体粪便中磺胺类药物的总浓度高达20 mg/kg。
