动物源性食品中青霉素类药物残留检测

建立动物源食品中同时检测4?种青霉素类药物残留的高效液相色谱法。以水合氨苄青霉素为内标，样品经乙腈-水（10∶1，V/V）提取，HLB固相萃取小柱净化。采用C18色谱柱，以0.02?mol/L磷酸二氢钾溶液-乙腈为流动相，梯度洗脱分离目标化合物进行定量分析。青霉素G、苯唑西林、乙氧萘青霉素、双氯青霉素在0.01～2?μg/mL范围内线性良好，线性相关系数均大于0.999，检出限和定量限分别为3?μg/kg和10?μg/kg；回收率在69.9%～100.3%之间，精密度的相对标准偏差在1.58%～9.15%之间。该方法前处理简单、快速、准确、灵敏，可以满足实际检测分析的需要。用于猪、牛、羊、鸡、鱼等不同基质中青霉素类药物残留的检测，取得了满意的结果。

Simultaneous Determination of Four Penicillin Residues in Animal Origin Foods

A high performance liquid chromatography (HPLC) method for the determination of four penicillin residues in foods of animal origin was developed.?Ampicillin trihydrate was used as the internal standard. Samples were extracted with a mixture of acetonitrile and water (10:1, V/V), and the extract was then cleaned up on an HLB solid-phase extraction cartridge. Penicillin G, oxacillin, nafcillin and dicloxacillin were separated on a C18 column by gradient elution with a mobile phase consisting of monopotassium phosphate (0.02 mol/L) and acetonitrile. The calibration curves were linear over the concentration range of 0.01–2 μg/mL with correlation coefficients of more than 0.999. The limits of detection (RSN > 3) (LOD) and quantification (RSN>10) (LOQ) were 3 and 10 μg/kg for all the analytes, respectively. The average recoveries were between 69.9% and 100.3% with relative standard deviations (RSDs) of 1.58%–9.15% (n = 6). The method is simple, rapid, sensitive and accurate and can meet the requirements for practical analysis. It has been applied with satisfactory results to detect penicillin residues in pork, beef, chicken and fish.