Yao Shanshan, Zhao Yonggang, Li Xiaoping, Chen Xiaohong, Jin Micong
Ningbo Municipal Center for Disease Control and Prevention, Ningbo Key Laboratory of Poison Research and Control, Ningbo 315010, China.
Se Pu. 2012 Jun;30(6):572-7. doi: 10.3724/sp.j.1123.2012.02014.
A method was developed for the determination of 11 anabolic hormones (boldenone, androstenedione, nandrolone, methandrostenolone, methyltestosterone, testosterone, testosterone acetate, trenbolone, testosterone propionate, stanozolol, fluoxymesterone) in fish by multi-function impurity adsorption solid-phase extraction-ultrafast liquid chromatography-tandem mass spectrometry. After the sample was extracted by methanol, the extract was cleaned-up quickly by C18 adsorbent, neutral alumina adsorbent and amino-functionalized nano-adsorbent. The separation was performed on a Shim-Pack XR-ODS II column (100 mm x 2.0 mm, 2.2 microm) using the mobile phases of 0.1% (v/v) formic acid in acetonitrile and 0.1% (v/v) formic acid solution in a gradient elution mode. The identification and quantification were achieved by using electrospray ionization in positive ion mode (ESI+) in multiple reaction monitoring (MRM) mode. The matrix-matched external standard calibration curves were used for quantitative determination. The results showed that the calibration curves were in good linearity for the eleven analytes with the correlation coefficients (r) more than 0.999. The limits of detection (LODs, S/N > 3) for the 11 anabolic hormones were from 0.03 microg/kg to 0.4 microg/kg and the limits of quantification (LOQs, S/N > 10) were from 0.1 microg/kg to 1.5 microg/kg. The average recoveries ranged from 80.9% to 98.1% with the relative standard deviations between 5.2% and 11.5%. The method is simple, rapid, sensitive, accurate and suitable for the quantitative determination and confirmation of the 11 anabolic hormones in fish.
建立了一种采用多功能杂质吸附固相萃取-超快速液相色谱-串联质谱法测定鱼类中11种同化激素（勃地龙、雄烯二酮、诺龙、美雄酮、甲基睾酮、睾酮、醋酸睾酮、群勃龙、丙酸睾酮、司坦唑醇、氟甲睾酮）的方法。样品经甲醇提取后，提取物通过C18吸附剂、中性氧化铝吸附剂和氨基功能化纳米吸附剂快速净化。在Shim-Pack XR-ODS II柱（100 mm×2.0 mm，2.2 µm）上进行分离，流动相为乙腈中0.1%（v/v）甲酸溶液和0.1%（v/v）甲酸溶液，采用梯度洗脱模式。在多反应监测（MRM）模式下，通过正离子模式（ESI+）的电喷雾电离进行鉴定和定量。采用基质匹配外标校准曲线进行定量测定。结果表明，11种分析物的校准曲线线性良好，相关系数（r）大于0.999。11种同化激素的检测限（LOD，S/N>3）为0.03 μg/kg至0.4 μg/kg，定量限（LOQ，S/N>10）为0.1 μg/kg至1.5 μg/kg。平均回收率为80.9%至98.1%，相对标准偏差为5.2%至11.5%。该方法简便、快速、灵敏、准确，适用于鱼类中11种同化激素的定量测定和确证。
