超高效液相色谱-串联质谱法测定肉类中的6种糖皮质激素

UPLC-MS/MS Determination of Glucocorticoids in Meat

为了准确测定肉类中的糖皮质激素含量,建立固相萃取-超高效液相色谱-串联质谱法分析测定肉类中的曲安西龙、氢化可的松、地塞米松、泼尼松、泼尼松龙和倍他米松6种糖皮质激素。样品经过提取后采用固相萃取法净化、富集,在负离子模式下采用MRM模式,采用BEH C18型色谱柱,以5 mmol/L甲酸铵和乙腈为流动相进行分离,并进行定性和定量分析,结果表明在10~200 ng/m L的质量浓度范围内,线性关系良好,相关系数在0.999 1~0.999 9。方法的检出限为0.1~0.3μg/kg,定量限为0.3~1.0μg/kg,回收率为84.3%~95.6%。

For the accurate determination of glucocorticoid in meat,a method was developed for the determination of the six glucocorticoids triamcinolone,hydrocortisone,dexamethasone,prednisone,prednisolone and betamethasone in meat by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry. After the extraction of samples,the solid phase extraction was used to clean up and enrich the samples. The target compounds were separated on a BEH C18 chromatographic column with 5 mmol/L ammonium formate-acetonitrile as mobile phase and detected in MRM mode via negative electrospray ionization（ESI-）,and carried out qualitative and quantitative analysis. The calibration curve showed a good linear from concentration 10~200 ng/m L with a correlation coefficient between 0.999 1~0.999 9. The detection limit of the developed method was 0.1~0.3 μg/kg and the quantification limit was 0.3~1.0 μg/kg. The average recovery rates were 84.3%~95.6%.