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建立了鸡肉组织中地塞米松、泼尼松、氢化可的松、甲基氢化泼尼松、曲安那德5种糖皮质激素的QuEChERS前处理方法以及超高效液相色谱-高分辨质谱(UHPLC-LTQ Orbitrap MS)检测方法。对QuECh-ERS前处理条件进行优化,结果表明,以乙酸乙酯为提取溶剂,乙二胺-N-丙基(PSA)为净化吸附剂,可达到最佳提取和净化效果。采用Waters AQUITY UPLC HSS T3(2.1 mm×150 mm,1.8μm)色谱柱进行分离,以乙腈-0.1%甲酸水溶液为流动相,梯度洗脱,流速为250μL/min。通过LTQ Orbitrap MS质谱检测器进行检测,以保留时间和精确质量数进行定性,母离子的峰面积进行定量。5种糖皮质激素的线性范围为1～100μg/L,相关系数均大于0.99,在5、10、20μg/kg 3个加标水平下的回收率为87.5%～119.7%,相对标准偏差(RSDs)为2.0%～11.0%。5种糖皮质激素的检出限(LODs)为0.49～0.78μg/kg,定量下限(LOQs)为1.62～2.57μg/kg。该方法稳定、可靠,可满足鸡肉中地塞米松等糖皮质激素残留的检测与确证要求。
A QuEChERS pretreatment method for dexamethasone, prednisone, hydrocortisone, methylprednisolone and triamcinolone acetate in chicken tissues was established and the effects of ultra-high performance liquid chromatography-high resolution mass spectrometry UHPLC-LTQ Orbitrap MS) detection method. The pretreatment conditions of QuECh-ERS were optimized. The results showed that ethylenediamine-N-propyl (PSA) could be used as purification adsorbent with ethyl acetate as extraction solvent to achieve the best extraction and purification effect. The separation was performed on a Waters AQUITY UPLC HSS T3 (2.1 mm × 150 mm, 1.8 μm) column using a gradient of acetonitrile-0.1% formic acid in water with a flow rate of 250 μL / min. Detected by the LTQ Orbitrap MS mass spectrometer, qualitatively characterized by retention time and accurate masses, the parent ion peak area was quantified. The linear range of the five glucocorticoids was 1 ~ 100μg / L, the correlation coefficient was greater than 0.99, and the recoveries were 87.5% ~ 119.7% at the three spiked levels of 5, 10 and 20μg / kg. The relative standard deviations ) Is 2.0% to 11.0%. The detection limits (LODs) of five glucocorticoids ranged from 0.49 to 0.78 μg / kg, and the LOQs ranged from 1.62 to 2.57 μg / kg. The method is stable and reliable, which can meet the requirements of detection and confirmation of dexamethasone and other glucocorticoid residues in chicken meat.