牛乳粉中氯霉素残留分析标准物质的定值方法研究及应用  

Research and application of the determination method of chloramphenicol residues reference material in milk powder

作　　者：成长玉 向琪 刘军 夏梦婷 郭庆 余晓琴 CHENG Changyu;XIANG Qi;LIU Jun;XIA Mengting;GUO Qing;YU Xiaoqin(Sichuan Institute of Food Inspection,Sichuan Chengdu 611731,China)

机构地区：[1]四川省食品检验研究院,四川成都611731

出　　处：《中国食品卫生杂志》2021年第6期755-759,共5页Chinese Journal of Food Hygiene

基　　金：国家重点研发计划项目(2017YFC1601300)。

摘　　要：目的建立一种基于液相色谱-串联质谱法的牛乳粉中氯霉素残留分析基体标准物质定值方法,并以此法用于该标准物质的均匀性、稳定性检验及定值。方法牛乳粉加水复原后,用乙酸乙酯提取,经正己烷除脂,再用乙酸乙酯萃取,同位素内标法定量测定。结果氯霉素在0.4~4.0 ng/mL范围内线性关系良好,相关系数达0.999,平均回收率为100.5%,相对标准偏差1.1%~3.2%(n=6),且该方法测定牛乳粉中氯霉素含量基质效应较弱。结论该方法准确、可靠,可用于标准物质定值;经11家实验室联合定值,牛乳粉中氯霉素残留分析标准物质的特性量值及其扩展不确定度(k=2)分别为(1.92±0.30)μg/kg和(5.65±0.53)μg/kg。Objective To establish a method for determination of the content of chloramphenicol in milk powder by liquid chromatography-mass spectrometry, and apply it to test the uniformity and stability of reference material and determine the value. Methods The milk powder was reconstituted by adding water, extracted with ethyl acetate, degreased with n-hexane, extracted with ethyl acetate again, and finally quantified by the isotope internal standard method. Results Chloramphenicol had a good linear relationship in the range of 0.4-4.0 ng/mL, the correlation coefficient was 0.999, the average recovery rate was 100.5%, the relative standard deviation was 1.1%-3.2%(n=6), and this method had a weak matrix effect in milk matrix. Conclusion The method is accurate and reliable, and can be used for the determination of reference materials. After jointly determination by 11 laboratories, the characteristic value and the expanded uncertainty(k=2) of the reference material for the analysis of chloramphenicol residues in milk powder are(1.92±0.30) μg/kg and(5.65±0.53) μg/kg.

关 键 词：牛乳粉 牛奶 氯霉素 标准物质 定值 

分 类 号：R155[医药卫生—营养与食品卫生学]