高效液相色谱法测定牛奶中硝基咪唑类残留量
高效液相色谱法测定牛奶中硝基咪唑类残留量
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。
ObjectiveTo establish a method for determination of nitroimidazoles (metronidazole, tinidazole and ornidazole) residues in milk by high performance liquid chromatography (HPLC). MethodsThe 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. ResultsMetronidazole, 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%. ConclusionThis method is simple and accurate, which is suitable for the determination of nitroimidazoles (metronidazole, tinidazole and ornidazole) residues in milk.
标题：高效液相色谱法测定牛奶中硝基咪唑类残留量
英文标题：Determination of nitroimidazoles residues in milk by high performance liquid chromatography
作者：
于敏 内蒙古蒙牛乳业(集团)股份有限公司
张美娟 内蒙古蒙牛乳业(集团)股份有限公司
张河霞 内蒙古蒙牛乳业(集团)股份有限公司
乌恩其木格 内蒙古蒙牛乳业(集团)股份有限公司
王丹慧 内蒙古蒙牛乳业(集团)股份有限公司
武慧明 内蒙古蒙牛乳业(集团)股份有限公司
秦培林 内蒙古蒙牛乳业(集团)股份有限公司
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,
发表日期：2017-10-13
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