高效液相色谱法测定牛奶中硝基咪唑类残留量

Determination of nitroimidazoles residues in milk by high performance liquid chromatography

中文关键词:  牛奶  硝基咪唑类  高效液相色谱法

英文关键词:milk  nitroimidazoles  high performance liquid chromatography

中文摘要:

      目的 建立高效液相色谱法检测牛奶中硝基咪唑类(甲硝唑、替硝唑、奥硝唑)残留。方法 试样经乙酸乙酯提取, 正己烷脱脂, 固相萃取柱净化, 以乙腈-乙酸缓冲液为流动相, C18反相色谱柱分离, 紫外检测器检测, 外标法定量。结果 甲硝唑、替硝唑、奥硝唑在0~1000.0 μg/kg范围内具有较好的线性关系, 相关系数(r2)大于0.998; 3种化合物检出限均为3 μg/kg, 定量限为10 μg/kg; 在10、50、100 μg/kg 3个添加水平回收率为73.8%~97.4%, 相对标准偏差为3.3%~9.5%。结论 该方法操作简单、准确性高, 适合于牛奶中硝基咪唑类(甲硝唑、替硝唑、奥硝唑)残留的检测。

英文摘要:

      Objective To establish a method for determination of nitroimidazoles (metronidazole, tinidazole and ornidazole) residues in milk by high performance liquid chromatography (HPLC). Methods The sample was extracted by ethyl acetate, defatted with n-hexane, and purified by solid phase extraction column. The acetonitrile acetic acid buffer was used as mobile phase, using C18 reversed phase chromatographic column separation and ultraviolet detector, and external standard method was used for quantitation. Results Metronidazole, tinidazole and ornidazole had good linear relationships in the range of 0~1000 μg/kg, and the correlation coefficients (r2)>0.998. The limits of detection and limits of quantification of 3 kinds of nitroimidazoles were 3 and 10 μg/kg, respectively. The recoveries spiked at 3 levels of 10, 50, 100 μg/kg were 73.8%~97.4%, and relative standard deviations (RSDs) were 3.3%~9.5%. Conclusion This method is simple and accurate, which is suitable for the determination of nitroimidazoles (metronidazole, tinidazole and ornidazole) residues in milk.