Screening and confirmation of steroids and nitroimidazoles in urine, blood, and food matrices: Sample preparation methods and liquid chromatography tandem mass spectrometric separations
Screening and confirmation of steroids and nitroimidazoles in urine, blood, and food matrices: Sample preparation methods and liquid chromatography tandem mass spectrometric separations
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DOI：
10.1016/j.jpba.2017.08.005
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发表时间：
2017-10
影响因子：
3.4
通讯作者：
Ádám Tölgyesi;Enikő Barta;A. Simon;T. McDonald;V. Sharma
中科院分区：
文献类型：
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作者：
Ádám Tölgyesi;Enikő Barta;A. Simon;T. McDonald;V. Sharma
含有合成合成代谢类固醇和硝基咪唑活性制剂的兽药不允许在欧盟（EU）的牲畜中使用。本文对12种类固醇和6种硝基咪唑类抗生素进行了低浓度（分别为1.56 μg/L ~ 4.95 μg/L和0.17 μg/kg ~ 2.14 μg/kg）的体液和卵子取样分析。分析包括清理程序、高效液相色谱（HPLC）分离、串联质谱筛选和验证方法。通过两种独立的固相萃取和液相萃取方法对样品中的靶类固醇和硝基咪唑进行清洗。所选化合物在Kinetex XB C-18高效液相色谱柱上进行梯度洗脱分离。筛选方法采用支持液体萃取，实现快速和经济有效的清理。通过增加基质和化合物的数量，以及引入同位素稀释质谱法对硝基咪唑的验证方法进行改进。根据欧盟参考实验室的建议，对新方法进行了验证，评估的性能特征完全符合标准。将该方法应用于能力测试中发生的样本。得到的z分数结果证明了所开发的方法对实际样本的适用性。将验证性方法应用于国家监测项目中，在少数尿样中检测到低浓度强的松龙的自然污染。
Veterinary drugs containing synthetic anabolic steroid and nitroimidazole active agents are not allowed for their applications in livestock of the European Union (EU). This paper presents analyses of twelve selected steroids and six nitroimidazole antibiotics at low levels (1.56 μg/L–4.95 μg/L and 0.17 μg/kg–2.14 μg/kg, respectively) in body fluids and egg incurred samples. Analyses involved clean-up procedures, high performance liquid chromatography (HPLC) separation, and tandem mass spectrometric screening and confirmatory methods. Target steroids and nitroimidazoles in samples were cleaned by two independent supported liquid extraction and solid phase extraction procedures. Separation of the selected compounds was conducted on Kinetex XB C-18 HPLC column using gradient elution. The screening methods utilised supported liquid extraction that enabled fast and cost effective clean-up. The confirmatory methods were improved by extending the number of matrices and compounds, and by introducing an isotope dilution mass spectrometry for nitroimidazoles. The new methods were validated according to the recommendation of the European Union Reference Laboratories and the performance characteristics evaluated met fully the criteria. The methods were applied to incurred samples in the proficiency tests. The obtained results of Z-scores demonstrated the applicability of developed protocols of the methods to real samples. The confirmatory methods were applied to the national monitoring program and natural contamination of prednisolone could be detected in urine at low concentration in few samples.