Captiva EMR-Lipid技术结合液相色谱-串联质谱法测定畜禽肉及内脏中4种抗生素残留

Determination of 4 kinds of antibiotics residues in meat and viscera of livestock and poultry by Captiva EMR-Lipid technology combined with liquid chromatography-tandem mass spectrometry

中文关键词:  液质联用法(HPLC-MS/MS)  抗生素  畜禽肉  固相萃取  兽药残留

英文关键词:liquid chromatography-tandem mass spectrometry  antibiotics  meat and viscera of livestock and poultry  solid phase extraction  veterinary drug residues

中文摘要:

      目的 建立液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry, LC-MS/MS)测定畜禽肉及内脏中4种抗生素(新生霉素、莫匹罗星、丰加霉素、茴香霉素)残留的检测方法。方法 样品经2%甲酸乙腈溶液提取和增强型脂质去除(Captiva EMR-Lipid)固相萃取柱净化, 采用Waters T3色谱柱分离目标物, 流动相以乙腈和含0.1%甲酸10 mmol/L甲酸铵水溶液梯度洗脱, 并采用电喷雾离子源的正离子扫描模式, 空白基质匹配外标法定量。结果 新生霉素、莫匹罗星、丰加霉素、茴香霉素在2.5~100.0 ng/mL范围内线性关系良好, 相关系数(r2)均大于0.9950。方法的检出限为1.0 μg/kg, 定量限为3.0 μg/kg。当加标回收实验的添加量为3.0~30.0 μg/kg时, 新生霉素、莫匹罗星、丰加霉素、茴香霉素加标回收率为76.3%~115.1%, 相对标准偏差均小于8% (n=6), 在猪肉基质中日内精密度和日间精密度均小于9% (n=5)。结论 本研究建立的检测方法, 样品前处理快速简便, 检测灵敏度高, 适用于市售畜禽肉及内脏中抗生素的风险筛查。

英文摘要:

      Objective To establish a method for the determination of 4 kinds of antibiotics (novobiocin, mupirocin, toyocamycin, and anisomycin) residues in meat and viscera of livestock and poultry by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods The samples were extracted with 2% formate acetonitrile solution, purified by enhanced matrix removal-lipid (Captiva EMR-Lipid) solid phase extraction column and separated by Waters T3 column. The mobile phase was eluted with a gradient of acetonitrile and 10 mmol/L formate ammonium aqueous solution containing 0.1% formic acid, the positive ion scanning mode of the electrospray ion source was used for quantitative detection, and blank matrix matching external standard method was used for analysis. Results The linear relationship between novobiocin, mupirocin, toyocamycin, and anisomycin was good in the range of 2.5–100.0 ng/mL, the correlation coefficient (r2) was greater than 0.9950. The detection limit was 1.0 μg/kg, and the quantitative limit was 3.0 μg/kg. The recovery rates of novobiocin, mupirocin, toyocamycin, anisomycin were 76.3%–115.1% when 3.0–30.0 μg/kg were added into the standard recovery experiment, the relative standard deviations were less than 8% (n=6), and the relative standard deviation s of intra-day and inter-day were less than 9% in the pork matrix (n=5). Conclusion The method established in this study is rapid, simple and sensitive, which is suitable for the risk screening of antibiotics in commercially available meat and viscera of livestock and poultry.