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采用超高效液相色谱-三重四极杆复合线性离子阱质谱仪(UPLCQTRAP),建立了动物组织中甲基睾酮、泼尼松龙、丙酸睾酮、群勃龙、睾酮、康力龙、美雄酮、诺龙和孕酮的测定方法。动物组织绞碎后添加Na2CO3均质,与硅藻土充分混合后填入空柱内,用20 m L叔丁基甲醚进行2次萃取,收集洗脱液,经旋转蒸发至干,用甲醇水溶液(1∶1,V/V)定容后测定。使用多反应监测(MRM)模式,确定检测离子对、进行数据采集。方法在1.0~100μg/L范围内线性关系良好,检出限(LOD)为0.04~0.19μg/kg,定量限(LOQ)为0.10~0.64μg/kg。在2~50μg/kg添加水平上,9种激素的平均回收率为73.3%~116.1%,相对标准偏差(RSDs)为3.4%~19%。方法适用于动物组织中甲基睾酮、泼尼松龙、丙酸睾酮、群勃龙、睾酮、康力龙、美雄酮、诺龙和孕酮等甾类同化激素的测定。
The effects of methyltestosterone, prednisolone, testosterone propionate, trabupram, testosterone, quetiapine, merostron, androsterone in animal tissues were established using ultra performance liquid chromatography-triple quadrupole linear ion trap mass spectrometry (UPLCQTRAP) Determination of nandrolone and progesterone. After homogenization, the animal tissue was homogenized with Na2CO3, thoroughly mixed with diatomaceous earth, filled into an empty column, extracted twice with 20 mL of tert-butyl methyl ether, and the eluate was collected and evaporated to dryness by rotary evaporation. 1: 1, V / V) after the determination of volume. Multiple reaction monitoring (MRM) mode was used to determine ion pairs for data acquisition. The method has good linearity in the range of 1.0 ~ 100μg / L with the limit of detection (LOD) of 0.04 ~ 0.19μg / kg and the limit of quantification (LOQ) of 0.10 ~ 0.64μg / kg. The average recoveries of nine hormones were 73.3% ~ 116.1% with relative standard deviations (RSDs) of 3.4% ~ 19% at the level of 2 ~ 50μg / kg. The method is suitable for the determination of steroid hormones such as methyltestosterone, prednisolone, testosterone propionate, racepone, testosterone, quetiapine, meloxerone, nandrolone and progesterone in animal tissues.