论文部分内容阅读
建立了测定罗非鱼肌肉中甲基睾丸酮残留的高效液相色谱-串联质谱(HPLC-MS/MS)方法。样品加乙醚超声振荡提取净化后,以乙腈-醋酸铵(5 mmoL)(75∶25,V/V)为流动相,流速250μL/min,经C18液相色谱柱分离后,进行串联质谱多反应检测模式下的定性和定量分析。采用电喷雾正离子模式检测,监测的离子对为m/z 303.4>m/z97.1,m/z303.4>m/z109.0。甲基睾丸酮的定量限为1.0μg/kg,线性范围为0.5~500 ng/mL,回收率范围为86.0%~112.0%,相对标准偏差值为0.7%~4.9%。研究表明,本方法具有灵敏度高、准确度高和精密度高等特点,适合罗非鱼肌肉中的甲基睾丸酮残留检测。
A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) method for the determination of methyltestosterone in muscle of tilapia was established. The sample was extracted with ether and extracted by ultrasonic wave. After the mobile phase was eluted with acetonitrile-ammonium acetate (5:50:50, V / V) and the flow rate was 250 μL / min, the sample was separated on a C18 column and subjected to tandem mass spectrometry Qualitative and Quantitative Analysis in Detection Mode. Using electrospray positive ion mode detection, the monitored ion pairs were m / z 303.4> m / z 97.1, m / z 303.4> m / z 109.0. The limit of quantitation of methyltestosterone was 1.0 μg / kg, the linear range was 0.5-500 ng / mL, the recovery range was 86.0% -112.0% and the relative standard deviation was 0.7% -4.9%. The research shows that this method has the characteristics of high sensitivity, high accuracy and high precision, and is suitable for the detection of methyltestosterone in the muscle of tilapia.