高效液相色谱法测定牛奶中硝基咪唑类残留量  被引量:19

Determination of nitroimidazoles residues in milk by high performance liquid chromatography

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作  者:于敏[1] 张美娟[1] 张河霞[1] 乌恩其木格 王丹慧[1] 武慧明 秦培林[1] 

机构地区:[1]内蒙古蒙牛乳业(集团)股份有限公司,呼和浩特011500

出  处:《食品安全质量检测学报》2018年第2期447-451,共5页Journal of Food Safety and Quality

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0~1000.0μg/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3μg/kg,定量限为10μg/kg;在10、50、100μg/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。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.

关 键 词:牛奶 硝基咪唑类 高效液相色谱法 

分 类 号:O657.72[理学—分析化学]

 

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