高效液相色谱-荧光检测法同时测定畜禽粪便中4种磺胺类药物残留

建立了高效液相色谱-荧光检测法测定畜禽粪便中4种磺胺药物(磺胺甲基嘧啶(SM1)、磺胺氯哒嗪(SCP)、磺胺邻二甲氧嘧啶(SDM’)、磺胺喹噁啉(SQ))的方法.样品用25 mL甲醇提取3次,合并提取液,浓缩干燥,用0.1 mol.L-1的HCL溶解残渣,经荧光胺衍生化后,用反相C18柱为分离柱,以乙腈∶0.5%乙酸=40∶60(V/V)为流动相进行洗脱,20 min内分离4种药物.在0.05—5.00μg.mL-1范围内,4种磺胺类药物的峰面积与质量浓度的线性关系良好(R2≥0.999),SM1、SCP、SDM’、SQ的定量限(LOQ)分别为2.3、6.3、4.3和9.6μg.kg-1;添加水平为50、100、1000μg.kg-1时,SM1、SCP、SDM’、SQ的回收率分别为74.91%—81.82%、78.45%—91.43%和86.10%—92.88%,RSD小于8.82%.

Simultaneous determination of four sulfonamide residue in the manure of livestock and poultry by HPLC with fluorescence detection

A method for the simultaneous determination of four sulfonamides(sulfamerazine(SM1),sulfachlorpyridazine(SCP),sulfadimoxine(SDM′),sulfaquinoxaline(SQ)) residues in manure of livestock and poultry was developed by using high performance liquid chromatography(HPLC) with fluorescence detection detector.The samples were extracted with 25 mL methanol for three times,and then the combined extracts were evaporated to dryness under reduced pressure at 45 ℃.The residue was dissolved in 0.1 mol · L-1 HCl and the analytes were derived with fluorescamine.The chromatographic separation was performed on a C18 column with a gradient elution program using a mixture of acetonitrile:0.5% acetic acid=40 ∶60 as mobile phase.The four sulfonamides were separated within 20 min.The calibration curve was linear in the range of 0.05—5.00 mg · L-1 and R2>0.999.The limit of quantification(LOQ) was 2.3,6.3,4.3 and 9.6 μg · kg-1 for SM1,SCP,SDM′ and SQ in manure of livestock and poultry.The recovery efficiencies were 74.91%— 81.82%,78.45%—91.43% and 86.10%—92.88%,with RSD <8.82%(n=5)at the spiking level of 50、100、1000 μg · kg-1,respectively.The method was suitable for the detection of SA residues in manure of livestock and poultry.