van Ginkel L A, Stephany R W, van Rossum H J, Steinbuch H M, Zomer G, Van de Heeft E, De Jong A P
National Institute of Public Health and Environmental Protection, Laboratory for Residue Analysis, Bilthoven, The Netherlands.
J Chromatogr. 1989 Apr 7;489(1):111-20. doi: 10.1016/s0378-4347(00)82888-1.
A method for the detection of nortestosterone (NT) in bovine muscle at levels below 1 microgram/kg is described, based on enzymatic digestion of the sample, clean-up by immunoaffinity chromatography after defatting and detection by gas chromatography-mass spectrometry (selected-ion monitoring). The immunoaffinity matrix was prepared after combining the isolated immunoglobulin G fractions from a rabbit antiserum raised against NT and methyltestosterone (MT). Its capacity per millilitre of gel was approximately 10 ng for each of the two steroids. Results for samples containing 0.1 microgram/kg NT and above are described. It is concluded that for multi-residue analysis of samples of muscle at levels as low as 0.1 microgram/kg, multi-immunoaffinity chromatography is a very suitable method of sample clean-up. For purposes of quantification the trideuterated internal standard [16,16,17 alpha-2H3] nortestosterone was synthesized.
本文描述了一种检测牛肌肉中含量低于1微克/千克的诺龙（NT）的方法，该方法基于样品的酶消化、脱脂后通过免疫亲和色谱法净化以及气相色谱-质谱联用（选择离子监测）进行检测。免疫亲和基质是在将从针对NT和甲基睾酮（MT）的兔抗血清中分离出的免疫球蛋白G组分结合后制备的。每毫升凝胶对这两种类固醇的容量约为10纳克。描述了含有0.1微克/千克及以上NT的样品的检测结果。得出的结论是，对于低至0.1微克/千克水平的肌肉样品进行多残留分析，多免疫亲和色谱法是一种非常合适的样品净化方法。为了进行定量，合成了氘代内标[16,16,17α-2H3]诺龙。
