基质分散固相萃取-高效液相色谱-可变波长检测法测定新鲜牛奶中8种抗生素

Determination of 8 kinds of antibiotics in fresh milk by matrix dispersion solid phase extraction-high performance liquid chromatography- variable wavelength detection method

中文关键词:  高效液相色谱法  抗生素  新鲜牛奶  基质分散固相萃取

英文关键词:high performance liquid chromatography  antibiotics  fresh milk  matrix dispersion solid phase extraction

中文摘要:

      目的 建立基于基质分散固相萃取-高效液相色谱-可变波长检测法测定新鲜牛奶中氯霉素、呋喃唑酮、甲硝唑、磺胺嘧啶、磺胺吡啶、磺胺-5-甲氧嘧啶、磺胺甲基异恶唑、磺胺二甲氧嘧啶8种抗生素的分析方法。方法 采用0.5%乙酸乙腈对新鲜牛奶中的8种抗生素进行提取, 提取液用C18粉末和乙二胺-N-丙基甲硅烷(primary secondary amine, PSA)粉末基质分散固相萃取, 以乙酸酸化的乙腈溶液(pH=3.0)和0.05 mol/L磷酸二氢钾溶液(pH=3.0)为流动相, Eclipse XDB-C18 (4.6 mm×150 mm, 5 μm)色谱柱, 梯度淋洗分离, 多波长检测定量。结果 8种抗生素在1.0~100.0 μg/kg质量浓度范围内线性关系良好, 相关系数为0.99904~1.00000; 对新鲜牛奶进行3个水平(5、20、50 μg/kg)的加标回收实验, 其回收率为84%~101%, 相对标准偏差为2.4%~10.7%; 检出限为0.18~0.41 μg/kg, 定量限为0.53~1.23 μg/kg。结论 本方法适用于新鲜牛奶或液态奶中抗生素的检测, 其前处理方法简便、回收率高、灵敏度高, 能够满足实验要求。

英文摘要:

      Objective To establish a method for the determination of 8 kinds of antibiotics [chloramphenicol (CAP), furazolidone (FZD), metronidazole (MNZ) and sulfadiazine (SD), sulfapyridine (SP), sulfamonomethoxine (SMM), sulfamethoxazole (SMX), sulfamethazine (SMZ)] in milk samples by matrix dispersion solid phase extraction-high performance liquid chromatography-variable wavelength detection method. Methods Eight kinds of antibiotics in fresh milk were extracted with 0.5% acetonitrile acetate. C18 powder and primary secondary amine (PSA) powder matrix were used for dispersive solid phase extraction. Acetonitrile solution acidified with acetic acid (pH=3.0) and 0.05 mol/L potassium dihydrogen phosphate (pH=3.0) were used as mobile phases. Eclipse XDB-C18 (4.6 mm×150 mm, 5 μm) was used as mobile phase chromatographic column, gradient elution separation, multi wavelength detection and quantification. Results Eight kinds of antibiotics wers good in the range of 1.0?100.0 μg/kg, the correlation coefficient was 0.99904?1.00000. The recoveries of 8 kinds of antibiotics at 3 spiked levels of 5, 20 and 50 μg/kg were ranged from 84% to 101%, and relative standard deviations ranging from 2.4% to 10.7%. The limits of detection (LOD) were 0.18 to 0.41 μg/kg, and the limits of quantification (LOQ) were between 0.53 to 1.23 μg/kg. Conclusion This method is suitable for the detection of antibiotics in liquid milk such as fresh milk. The method is simple, with high recovery rate and sensitivity, and can meet the requirements of the experiment.