Analytical Biosciences, Department of Pharmacy, Faculty of Health and Medical Sciences, University of Copenhagen, Universitetsparken 2, 2100 Copenhagen, Denmark.
J Chromatogr A. 2013 Sep 13;1307:27-33. doi: 10.1016/j.chroma.2013.07.062. Epub 2013 Jul 19.
A multi-residue pressurised liquid extraction (PLE) methodology has been established for the determination of the four ionophores: lasalocid, monensin, salinomycin and narasin in solid environmental matrices. The PLE methodology is combined with solid phase extraction as clean-up using liquid chromatography coupled to tandem mass spectrometry applying electrospray ionisation for detection. The samples were freeze-dried prior to extraction. The absolute recoveries for soil and sediment ranged from 71 to 123% (relative standard deviation (RSDs) below 16%) and in the range 94-133% (RSDs 9-35%) for poultry manure. The final method allowed for the detection of four ionophores down to a few hundred ngkg(-1) in natural solid matrices with limit of quantifications (LOQs) being 0.96, 0.87, 0.98, and 0.64μgkg(-1) in soil for lasalocid, monensin, salinomycin, and narasin, respectively. Corresponding LOQs in sediment were 1.28, 1.34, 1.39, and 0.78μgkg(-1) for the respective ionophores, while in manure the LOQs were 0.98, 1.01, 1.45, and 1.01μgkg(-1).
建立了一种用于测定固体环境基质中 4 种离子载体：拉沙里菌素、莫能菌素、盐霉素和那拉菌素的多残留加压液体萃取（PLE）方法。该 PLE 方法与固相萃取相结合，采用液相色谱-串联质谱法，电喷雾电离作为检测手段，进行净化。在提取前，将样品冷冻干燥。土壤和沉积物的绝对回收率在 71%至 123%之间（相对标准偏差（RSD）低于 16%），禽粪的回收率在 94%至 133%之间（RSD 为 9%至 35%）。最终方法允许在自然固体基质中检测到四种离子载体，其浓度低至数百纳克/千克（ng/kg），土壤中拉沙里菌素、莫能菌素、盐霉素和那拉菌素的定量限（LOQs）分别为 0.96、0.87、0.98 和 0.64μg/kg，沉积物中的 LOQs 分别为 1.28、1.34、1.39 和 0.78μg/kg，禽粪中的 LOQs 分别为 0.98、1.01、1.45 和 1.01μg/kg。
