固相萃取-高效液相色谱法测定猪组织中的头孢喹诺

Determination of Cefquinome in Porcine Tissues by Solid Phase Extraction-High Performance Liquid Chromatography

本文建立了固相萃取-高效液相色谱法测定猪组织中头孢喹诺的方法。组织样品用磷酸盐缓冲液、异辛烷和乙腈提取,40℃旋转蒸发至近干,C18固相萃取小柱净化后注入高效液相色谱仪分析。采用Inertsil C18色谱柱（250×4.6 mm,5μm）,以磷酸盐缓冲液-乙腈（体积比为80∶20）为流动相,于270 nm波长处检测。肌肉、脂肪、肝脏和肾脏样品中头孢喹诺的检测限分别为5、10、15、30μg/kg。在20~2 000μg/kg添加水平内,平均回收率为55.7%~79.4%,相对标准偏差为3.3%~5.7%。本方法可用于猪组织中头孢喹诺残留的检测。

A solid phase extraction and high performance liquid chromatography（SPE-HPLC） method was developed for the determination of cefquinome in porcine tissues.Porcine tissues were extracted by phosphate buffer,isooctane,and acetonitrile.The extract was blowed with rotating evaporation under 40℃ until it was rearly dry,then passed through preconditioned C18 solid phase extraction cartridge.HPLC analysis was carried out using a Inertsil C18 column（250×4.6 mm,5 μm） with ultraviolet detector at a wavelength of 270 nm.The mobile phase was a mixture of phosphate buffer and acetonitrile（80∶20）.The column temperature was 25℃.The injection volume was 100 μL.The limit of detection of the method was 5 ng/g for muscle,10 ng/g for fat,15 ng/g for liver and 30 ng/g for kidney.Average recovery at a spiking concentration range of 0.02～2.0 μg/g were 55.7%～79.4%,and the relative standard deviations were 3.3%～5.7%.The results indicate that the method is suitable for the determination of cefquinome residue in porcine tissues.