UHPLC-LTQ Orbitrap MS测定鸡肉组织中5种糖皮质激素残留

Determination of 5 Glucocorticoids Residues in Chicken Muscle Tissue by Ultra High Performance Liquid Chromatography LTQ Orbitrap Mass Spectrometry

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 sample pretreatment coupled with ultra high performance liquid chromatogra phy - LTQ Orbitrap mass spectrometric （ UHPLC - LTQ Orbitrap MS） method was developed for the sim uhaneous determination of 5 glucocorticoids residues, including dexamethasone, prednisone, hydro cortisone, methylprednisolone and tiramacinolone, in chicken muscle tissues. The QuEChERS pretreat ment procedure was optimized. The chicken muscle samples were extracted with ethyl acetate and cleaned by PSA dispersive solid phase extraction. The separation of target compounds was performed on a Waters AQUITY UPLC HSS T3（2. 1 mm x 150 mm, 1.8 μm） column by gradient elution using ace tonitrile -water（containing 0. 1% formic acid） as mobile phase at a flow rate of 0. 25 mL/min. Identi fication of the glucocorticoids was based on the retention time and the exact mass of [ M ＋ H ] ^＋ ions, and quantification of the glucocorticoids was based on the peak area of [ M ＋ H ] ^＋ ions. The linear ran- ges of five compounds were in the range of 1 - 100 μg/L, with correlation coefficients more than 0. 99. The average recoveries of 5 glucocorticoids at spiked levels of 5, 10, 20 μg/kg ranged from 87. 5% to 119. 7% , with relative standard deviations（RSDs） of 2. 0% -11.0%. The limits of detection（LODs）of the method ranged from 0. 49 μg/kg to 0. 78 μg/kg, and the limits of quantitation （LOQs） ranged from 1.62 μg/kg to 2, 57 μg/kg. The method was reliable and efficient, and could be applied in the determination of 5 glucocorticoids in chicken muscle samples.