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目的:建立马尿中32种蛋白同化激素的液相色谱串联质谱(LC-MS/MS)检测方法。方法:利用Agilent 6410A LC-MS/MS仪器;色谱柱采用Agilent Zorbax XDB-C18柱(2.1×100 mm,3.5μm);流动相采用0.1%甲酸水溶液(A)和乙腈(B)进行梯度洗脱;离子检测方式为多反应离子检测(MRM);正离子检测。结果:建立了马尿中32种蛋白同化激素的检测方法,药物浓度线性方程的相关系数均大于0.992,日内和日间精密度基本小于20%,提取回收率在84%以上且基质效应多在80%~120%之间,LOD和LOQ满足相关马术检测机构的要求。结论:本方法操作简单,经方法学验证符合相关标准,能满足马术项目的兴奋剂检查要求,可以应用于常规的兴奋剂检测。
Objective: To establish a liquid chromatography tandem mass spectrometry (LC-MS / MS) method for the determination of 32 protein anabolic hormones in horse urine. Methods: The Agilent 6410A LC-MS / MS instrument was used. The column was equipped with an Agilent Zorbax XDB-C18 column (2.1 × 100 mm, 3.5 μm). The mobile phase was eluted with a gradient of 0.1% formic acid in water ; Ion detection for multiple reaction detection (MRM); positive ion detection. Results: The method for determination of 32 protein anabolic hormones in mare was established. The correlation coefficient of the linear equation of drug concentration was greater than 0.992. The intra- and inter-day precision was less than 20%. The extraction recovery was above 84% 80% ~ 120%, LOD and LOQ meet the requirements of the relevant equestrian testing agencies. Conclusion: The method is easy to operate and verified by methodological validation in accordance with relevant standards. It can meet the requirements of doping control of equestrian projects and can be applied to conventional doping detection.