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采用液相色谱-四极杆/离子阱质谱(LC-Q/Trap-MS)建立了肌肉中16种同化甾体激素类物质(ASs)残留的同时确证及测定方法。肌肉中的ASs采用乙腈超声辅助提取,正己烷脱脂,氨基固相萃取柱净化,CAPCELL PAK C18MGⅢ柱(150 mm×2.0 mm,5.0μm)分离,0.1%(v/v)甲酸-乙腈溶液和0.1%(v/v)甲酸-5 mmol/L甲酸铵水溶液为流动相梯度洗脱;预设定多反应监测(sMRM)-信息依赖性采集(IDA)-增强子离子扫描(EPI)模式检测,在线EPI谱库确证,内标法定量。结果表明,16种ASs在线性范围内线性关系良好(r≥0.999);定量限(LOQ,S/N≥10)为0.029～0.36μg/kg;3个添加水平(0.5、2.0和20μg/kg)下的回收率为89.9%～118%;相对标准偏差(RSD)为6.3%～16.2%。该方法准确灵敏,一次性完成16种ASs的确证和测定,可有效用于肌肉组织中ASs残留的监测分析。
Simultaneous confirmation and determination of residues of 16 kinds of anabolic steroid substances (ASs) in muscle were established by liquid chromatography-quadrupole / ion trap mass spectrometry (LC-Q / Trap-MS) ASs in muscle were extracted with acetonitrile, degreased with n-hexane and cleaned up with a solid-phase extraction column on a CAPCELL PAK C18MGIII column (150 mm × 2.0 mm, 5.0 μm). 0.1% (v / v) formic acid- 5 mmol / L ammonium formate in aqueous solution of 5% (v / v) formic acid as mobile phase gradient elution; pre-defined multiple reaction monitoring (sMRM) -information dependent acquisition (IDA) -concentrator ion scan (EPI) Online EPI library confirmation, internal standard method. The results showed that the 16 ASs had a good linearity (r ≥0.999) in the linear range, the limits of quantitation (LOQ, S / N≥10) were 0.029-0.36μg / kg, and the three addition levels were 0.5,2.0 and 20μg / kg ) Was 89.9% ~ 118%. The relative standard deviation (RSD) was 6.3% ~ 16.2%. The method is accurate and sensitive, confirming and measuring 16 ASs in one time, and can be effectively used for the monitoring and analysis of ASs residues in muscle tissues.