快速高分离液相色谱-串联质谱法对肌肉组织中糖皮质激素残留的检测

Determination of Glucocorticoid Residues in Animal Muscle by Rapid Resolution Liquid Chromatography-Tandem Mass Spectrometry

建立采用快速高分离液相色谱-串联质谱(UHPLC-MS2)技术检测肌肉组织中糖皮质激素残留的方法。样品经乙酸乙酯提取,固相萃取法净化,以C18色谱柱(150mm×2.1mm,3.5μm)为分离柱,水-乙腈-甲酸溶液为流动相进行梯度洗脱,快速高分离液相色谱-串联质谱ESI负离子模式进行检测。该方法线性范围为0.5～5ng/mL,线性相关系数R2≥0.9963,检测限:倍氯米松为1.0μg/kg,氢化可的松为2.0μg/kg,其余均为0.5μg/kg。平均回收率为82.75%～91.87%,相对标准偏差≤4.43%(n=5)。

A method was developed for the determination of seven glucocorticoid residues in animal muscle using liquid chromatography-tandem mass spectrometry （LC-MS/MS）. Sample extraction was performed using ethyl acetate,followed by cleanup based on solid phase extraction （SPE）. The chromatographic separation was achieved on a C18 column （150 mm × 2.1 mm,3.5 μ m） with water/acetonitrile/formic acid system as the mobile phase in gradient elution mode. The MS condition used was negative electrospray ionization mode. Under these conditions,the linear range of the developed method was between 0.5 ng/mL and 5 ng/mL,with a linear correlation coefficient of no less than 0.9963,the detection limit was 1.0μg/kg for beclomethasone,2.0 μg/kg for hydrocortisone,0.5μg/kg for the others,and the average spike recoveries for the seven molecules were between 82.75% and 91.87%,with a relative standard deviation （RSD） of 4.43% or lower （n = 5）.