HPLC法测定肉中五种磺胺兽药残留量及其不确定度评估

Determination of 5 sulfonamides residues by high performance liquid chromatography in meat

〔目的〕建立肉中 5种磺胺兽药残留量测定方法。〔方法〕采用高效液相色谱 (HPLC)梯度洗脱法同时测定肉中磺胺嘧啶、磺胺二甲嘧啶、磺胺 - 5 -甲氧嘧啶、磺胺二甲氧嘧啶、磺胺喹恶啉残留量。使用Capcell-pakC18柱 (SHISEI DO) ,以乙腈和 1% (V/V)乙酸溶液为流动相 ,使用紫外检测器 ,在 2 70nm处对样品中 5种磺胺兽药进行检测。〔结果〕磺胺嘧啶、磺胺二甲嘧啶、磺胺 - 5 -甲氧嘧啶、磺胺二甲氧嘧啶、磺胺喹恶啉分别在 0 196 μg/ml～ 1 96 4 μg/ml,0 199μg/ml～1 992 μg/ml,0 2 2 0 μg/ml～ 2 2 0 4 μg/ml,0 188μg/ml～ 1 884 μg/ml,0 2 0 4 μg/ml～ 2 0 36 μg/ml范围内有良好的线性关系 ,其线性相关系数分别为r=0 9989,r=0 9990 ,r=0 9993,r=0 9993和r=0 9991;回收率在 72 2 3%～ 93 75 %。〔结论〕该方法专属性强、灵敏可靠、重现性好。

睴bjective〕To analyze 5 Sulfonamides residues in meat 〔Methods〕 HPLC method with gradient elution was developed to separate and determine Sulfadiazine, Sulfadimidine,Sulfameth-oxydiazine,Sulfadimoxinum, Sulfquinoxaline residues in meat on Capcell-pak C 18 column,using acetonitrile-acetic solution(1%) as mobile phase Detection was performed with UV detector at 270nm 〔Results〕The calibration curves were linear within the ranges of 0 196μg/ml～1 964μg/ml for Sulfadiazine ( r =0 9989),0 199μg/ml～1 992μg/ml for Sulfadimidine( r =0 9990), 0 220μg/ml～2 204μg/ml for Sulfamethoxydiazine ( r =0 9993),0 188 μg/m～1 884μg/ml for Sulfadimoxinum( r =0 9993),0 204μg/ml～2 036μg/ml for Sulfquinoxaline ( r =0 9991);The recoveries and RSDs were 93 75% and 4 81% for Sulfadiazine, 91 01% and 5 01% for Sulfadimidine, 89 77% and 5 39% for Sulfamethoxydiazine , 77 49% and 5 90% for Sulfadimoxinum, 72 23% and 7 28% for Sulfquinoxaline 〔Conclusions〕 That this method is specific,accurate,reproducible