QuEChERS/液相色谱-串联质谱法同时测定鱼肉中30种激素类及氯霉素类药物残留

建立了鱼肉中8种雌激素、5种雄激素、6种孕激素、8种糖皮质激素及3种氯霉素类药物多残留的QuEChERS/液相色谱-串联质谱(LC - MS/MS)同时测定方法.均质样品用水分散后加乙腈提取,经分散固相萃取净化后,采用ZORBAX Extend-C18色谱柱(100 mm ×2.1 mm,3.5 μm)分离,分别在电喷...     

肉食品中常见4种抗生素残留的高效液相色谱分析

建立了同时测定肉食品中泰乐菌素、替米考星、氯霉素、氟苯尼考的高效液相色谱方法,样品经乙腈提取,正己烷脱脂, HLB小柱净化后,以C18反相色谱柱为分离柱,甲醇－磷酸二氢钠缓冲溶液(pH 3.0,含体积比为10％的甲醇溶液）为流动相进行梯度洗脱,检测波长λ为275 nm.泰乐菌素、替米考星、氯霉素、氟苯尼考的线性范围是0.1～20.0 mg/L,相关系数分别为0.9987、0.9992、0.9985、0.9970.其平均回收率为75％～87%,相对标准偏差为1.35％～5.41％,泰乐菌素、替米考星、氯霉素、氟苯尼考的检出限分别为20、32、19、16μg/kg.方法满足肉食品中泰乐菌素、替米考星、氯霉素、氟苯尼考的残留量测定.     

超高效液相色谱-串联质谱法同时测定牛奶中38种抗生素残留

建立了超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定牛奶中5类(磺胺类、喹诺酮类、四环素类、氯霉素类和大环内酯类)38种抗生素的分析方法。牛奶样品以0.5%(体积分数)甲酸乙腈提取,利用Oasis PRiME HLB固相萃取小柱进行净化,经Acquity UPLC HSS T3柱(100 mm×2.1 mm i.d.,1.8μm)分离,采用电喷雾离子源,多反应监测模式(MRM)进行定性定量分析。结果表明,38种抗生素在各自线性范围内呈良好的线性关系,相关系数(r~2)均大于0.99,定量下限为0.10～1.0μg/kg;在1.0、5.0、10.0μg/kg加标水平下,平均回收率为70.7%～94.9%,相对标准偏差(RSD,n=6)为4.0%～9.4%。该方法操作简单、灵敏度高、重现性好,适用于牛奶中多种抗生素残留的监测要求。     

Analysis of antibiotics from liquid sample using electrospray ionization-ion mobility spectrometry

The recent findings of antibiotic residues in aquatic environment at trace level have gained much concern for the detrimental effect on ecological and human health due to bacterial resistance. Here, the feasibility of using electrospray ionization ion mobility spectrometry (ESI-IMS) for analysis antibiotics in liquid sample is demonstrated. Reduced mobilities and collision cross sections of 18 antibiotics are experimentally measured and compared with theoretical values according to mass-mobility correlation. Gentamicin is used as an example to investigate the capability of ESI-IMS for multi-component analysis of antibiotics. Mixtures of antibiotics at different concentrations are analyzed. The estimated detection limit for amoxicillin is 0.7 mg L⁻¹ (70 pg) and the linear range of response maintains over two orders. This method will be a potential technique for the analysis of antibiotics in aquatic environment.