摘要
采用高效液相色谱法测定牛、猪肌肉和肾脏中头孢噻呋相关残留量。样品经二硫赤藓糖醇溶液提取,碘乙酰胺衍生,固相萃取柱(C18、SAX和SCX)净化,C18柱色谱分离,以乙腈-水(体积比15:85)含0.1%三氟乙酸作流动相等梯度洗脱,266nm紫外检测。头孢噻呋残留量在0.016~1.28mg/L范围内与峰面积呈良好线性,相关系数r〉0.9999。样品添加浓度在200~8000μg/kg的回收率为90%~91%,相对标准偏差为1.8%-3.5%。本方法的检出限(信噪比S/N=3)为50μg/kg。
Ceftiofur related residues in bovine and porcine muscle and kidney were determined by high performance liquid chromatography. Samples were extracted with dithioerythritol, derivatized with iodoacetamide and cleaned up on C18, SAX and SCX solid-phase extraction cartridges. Chromatographic separation was carried out on a C18 column (250 mm×4.6 mm, 5 μm) with acetonitrile - water (15 : 85 by volume) containing 0. 1% trifluoroacetic acid as mobile phase at a flow rate of 1 mL/min, followed by determination of the residue by ultraviolet absorption detector at 266 nm. Calibration curve was linear between 0. 016 and 1.28 mg/L, with the correlation coefficient r 〉 0. 999 9. The recovery and relative standard deviation ranged from 90% to 91% and 1.8% to 3.5% at spiked level of 200 - 8 000 μg/kg, respectively. The detection limit of the proposed method was 50 μg/kg.
出处
《分析测试学报》
CAS
CSCD
北大核心
2008年第2期178-180,184,共4页
Journal of Instrumental Analysis