亚临界流体萃取高效液相色谱法测定鱼肉中丙酸睾酮残留

采用亚临界1,1,1,2-四氟乙烷(R134a)萃取技术作为样品的前处理技术,建立亚临界流体萃取高效液相色谱法测定鱼肉中丙酸睾酮残留量的新方法。在对添加了丙酸睾酮的罗非鱼肌肉样品亚临界R134a萃取单因素实验的基础上,通过正交实验对萃取条件进行了优化,结果为:萃取压力14MPa,萃取温度23℃,R134a流量1.0L/min(标态),静态萃取30min,动态萃取40min,共溶剂甲醇添加量2mL,收集液为甲醇。收集液经石油醚纯化后,用高效液相色谱检测。在最优条件下,方法回收率大于90%、相对标准偏差(RSD)小于5%。最后,对实际样品进行实际检测,鱼肉冷冻干燥样品中丙酸睾酮的残留量为1.37μg/g。本方法首次利用亚临界R134a萃取作为兽药残留分析样品的前处理技术,萃取压力和萃取温度都比较低,易于大规模推广应用。

Determination of Testosterone Propionate Residues in Aquatic Products Using Subcritical 1,1,1,2-tetrafluoroethane(R134a) Extraction and Liquid Chromatography

Using Subcritical 1,1,1,2-tetrafluoroethane(R134a) extraction as sample preparation technique,a new subcritical fluid extraction-liquid chromatography method for determination of testosterone propionate residues in aquatic products was developed.Tilapia muscle fortified with testosterone propionate was dealt with subcritical R134a extraction,and on the basis of single factor experiments,orthogonal design experiments was used to optimize the effecting factors.The optimized extracting conditions were as follows: pressure 14 MPa,temperature 23 ℃,static extraction time 20 min,dynamic extraction time 40 min,cosolvent 2 mL methanol,and 1.0 L/min R134a flow.Methanol was used as collecting solvent,and the residues were purified by liquid-liquid extraction with petroleumether and determined by HPLC.The average recovery of testosterone propionate was greater than 90%,and the RSD were less than 5%.Finally,the positive tissue control was measured in practice,and the residue of testosterone propionate was 1.37μg/g.It is for the first time at home and abroad that subcritical R134a extraction was used as pretreatment technology for residue analysis.And subcritical R134a extraction has low extraction pressure and temperature,so it can be applied in large-scale application.