水产品中四环素类抗生素残留量的高效液相色谱测定方法

本文建立了高效液相色谱(HPLC)检测水产品中3种四环素类抗生素残留量的方法。采用4%高氯酸溶液提取样品中的残留抗生素,经浓缩处理,以乙氰和0.01mol·L-1NaH2PO4(18∶82,v/v)为流动相,流速1mL·min-1,3种抗生素组分峰能与杂质峰完全分开,检测波长为355mm。在50~1000μg·mL-1范围内,峰面积与抗生素浓度呈良好的线性关系(r2>0.99),以测量的3倍标准偏差计算方法的检出限分别为0.045μg·g-1(土霉素)、0.041μg·g-1(四环素)和0.080μg·g-1(金霉素)。平均加标加收率分别为96.5%(土霉素)、87%(四环素)和73.2(金霉素)。精密度(RSD)小于5%。实验检测了几种常见水产品样品的四环素类抗生素残留量,发现在本检出水平下被检测的几种鱼和虾样品均未能检出。

Determination of tetracycline antibiotic residucs in aquiculturc products by HPLC

The residues of tetracycline antibiotics including oxytetracycline (OTC),tetracycline (TC) and chlortetracycline (CTC) in several kinds of aquiculture products were measured with the optimized method of high performance liquid chromatography (HPLC).The tetracycline antibiotics in seafood samples were extracted twice by 4% HClO_4,and the combined extracts were concentrated till dryness in 70℃ water bath under a gentle stream of nitrogen.Then,its residue was resolved in 4% HClO_4 and the solutions were filtrated with 0.45μm membrane.The tetracycline antibiotic samples were separated by the RP-HPLC column (Waters 3.6mm×15cm,4.6μm)with a mobile phase of acetonitrile and 0.01mol·L -1NaH_2PO_4(18∶82,v/v) at the rate of 1 mL/min and detected at 355 nm.The average recoveries tested with adding standards were 96.5% for OTC,87% for TC and 73.2% for CTC,and the detection limit estimated with 3 -fold standard deviation was 0.045μg·g -1 for OTC,0.041μg·g -1for CTC and 0.080μg·g -1for CTC,respectively. The three kinds of tetracycline antibiotics in actual aquiculture products could not be detected with the established method.