高效液相色谱法检测鸡蛋中四环素类药物残留方法研究

试验旨在建立同时检测鸡蛋中土霉素、四环素、金霉素和多西环素4种四环素类药物残留的高效液相色谱法。将鸡蛋样品用0.1 mol/L Na₂EDTA-Mcllvaine缓冲溶液提取,通过Oasis MAX固相萃取柱净化,以乙腈—三氟乙酸(0.01 mol/mL)为流动相,梯度洗脱,反相液相色谱分离测定。结果显示,4种四环素类药物在30~1 000 ng/g范围内呈良好线性关系,检出限为10 ng/g,定量限为50 ng/g,平均回收率为67.3%~81.4%,日内相对标准偏差为2.7%~14.3%,日间相对标准偏差为0.9%~5.0%。本研究建立的高效液相色谱法可同时检测鸡蛋中的土霉素、四环素、金霉素和多西环素的药物残留,该方法灵敏度、准确度和精密度较高,操作快速、简单。

Residue Detection of Tetracyclines in Eggs by High Performance Liquid Chromatography

The study was aimed to establish the method of simultaneous detection of four kinds of tetracyclines,including oxytraoycline,tetracycline,chlortetracycline and doxyeycline in eggs by high performance liquid chromatography (HPLC).The eggs samples were detected with HPLC after through the procedure of extraction of 0.1 mol/L Na₂EDTA-Mcllvaine buffered solution,purification of Oasis MAX solid-phase extraction column,gradient elution of taking acetonitrile-0.01 mol/mL trifluoroacetic acid as mobile phase,separation with reverse liquid chromatography.The results showed that the calibration curves of four kinds of tetracyclines were linear correlated in the concentration range of 30 to 1 000 ng/g which the limits of detection was 10 ng/g and the limit of quantification was 50 ng/g.The average recoveries were 67.3% to 81.4%,relative standard deviations of intraday was 2.7% to 14.3%,relative standard deviations of inter-day was 0.9% to 5.0%.This mothod established in this study could simultaneously detect oxytetracycline,tetracycline,chlortetracycline and doxycycline drug residues in egg and it had high sensitivity,accuracy and precision.The method was rapid and simple to operate.