摘要
建立了猪肉和牛奶中磺胺嘧啶(SD)、磺胺噻唑(ST)、磺胺二甲嘧啶(SM2)、磺胺甲氧嗪(SMP)、磺胺氯哒嗪(SPD)、磺胺间甲氧嘧啶(SMM)、磺胺甲基异嗯唑(SM2)、磺胺氯吡嗪(Esb3)、磺胺地索辛(SDM)和磺胺喹嗯啉(SQ)共10种磺胺类药物残留检测的超高效液相色谱(UPLC)法。色谱条件:色谱柱为Acquity UPLC BEH C18柱(2.1mm×50mm,1.7μm);流动相为50%甲醇乙腈溶液-2%乙酸水溶液,梯度洗脱;紫外检测波长270nm;柱温30℃;进样量4μL;外标法定量。结果表明:10种组分在20~1000ng/mL浓度范围内,呈良好线性关系,相关系数R^2均大于0.998;方法检出限为20ng/g,定量限为50ng/g;在猪肉和牛奶中添加浓度分别为50、100、200ng/g时,平均回收率为75.1%~99.8%,批内、批间平均RSD均小于13.2%。
A UPLC method was established for ten sulfonamides including sulfadiazine (SD), sulfathiazole (ST), sulfadimidine( SM2 ), sulfamethoxypyridazine (SMP) , sulfachlorpyridazine ( SPD), sulfamonomethoxine ( SMM ), sulfamethoxazole (SMZ), sulfachloropyrazine ( Esb3 ), sulfadimethoxine (SDM) and sulfaquinoxaline (SQ) in pig muscle and milk. UPLC conditions:the chromatography column was Acquity UPLC BEH Cls column of 2.1 mm × 50 mm, 1. 7 μm;mobile phase was acetonitrile - methanol( 1 : 1, V/V) - water(2% acetic acid) ; Column temperature was 30 ℃ ; Determination was by UV detection at 270 nm; Injection volume is 4 μL. The calibration curve was good linear between the peak areas and concentrations of sulfonamides from 20 to 1 000 ng/mL, the correlation coefficient R^2 〉 0.998. The limit of detection was 20 ng/g; The limit of quantification was 50 ng/g. The average recoveries from spiked pig muscle and milk at the three concentrations of 50, 100 and 200 ng/g ranged from 75.1% -99.8% ,and intra- day and interday(n=5) batch variation coefficients were less than 13.2%.
出处
《中国兽药杂志》
2009年第8期1-4,17,共5页
Chinese Journal of Veterinary Drug