猪肉和牛奶中10种磺胺类药物残留检测超高效液相色谱法研究

Simultaneous Determination of Ten Sulfonamides Residues in Pig Muscle and Milk by UPLC

关键词:  猪肉  牛奶  磺胺类药物  残留  UPLC

Key words:  pig muscle  milk  sulfonamides drugs  residue  UPLC

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）、磺胺甲基异噁唑（SMZ）、磺胺氯吡嗪（Esb3）、磺胺地索辛（SDM）和磺胺喹噁啉（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 (2.1×50mm,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R2均>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%。

Abstract:

A UPLC method was established for the 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 C18 column of 2.1×50mm，1.7µm；mobile phase was acetonitrile –methanol(1:1，V/V)-water(2% acetic acid)；Column temperature was 30℃；Determination was by UV detection at 270nm;Injection volume is 4µL. The calibration curve was good linear between the peak areas and concentrations of sulfonamides from 20 to 1000ng/mL,the correlation coefficient R2>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 inter-day（n=5） batch variation coefficients were less than 13.2%.