摘要
建立食品中四种新型那非衍生物的高效液相色谱串联质谱分析方法。样品经甲醇超声提取,提取液离心过膜后上机分析。采用C18色谱柱(2.1 mm×50 mm,1.7μm)分离,以0.1%甲酸水溶液和乙腈为流动相进行梯度洗脱,外标法定量测定。四种新型那非衍生物在1~50 ng/mL的范围内线性关系良好,相关系数均高于0.995,检出限均为0.05 mg/kg,定量限均为0.1mg/kg。四种新型那非衍生物于1、2、10倍定量限3个水平下的平均加标回收率范围为80.13~105.97%,相对标准偏差(RSD)范围为0.11~7.75%。采用该方法对收集的121批次样品进行分析,共检出17批次阳性样品,含量范围为27.92~5910 mg/kg。该方法高效准确,满足食品中非法添加四种新型卡巴地那非衍生物的定性定量分析,有效填补食品中这四种新型非法添加那非类物质监管空白。
To establish a high-performance liquid chromatography tandem mass spectrometry method for the analysis of four novel nafil derivatives in food.The sample was extracted by methanol ultrasound,the extract was centrifuged,filtered through a microporous membrane,and analyzed by the high-performance liquid chromatography-mass spectrometry.The separation was performed on a Cis column(2.1 mmx50 mm,1.7μm)with gradient elution by using 0.1% formic acid aqueous solution and acetonitrile as the mobile phase,and quantified by extermal standard method.The four novel nafil derivatives demonstrated good linearity in the range of 1~50 ng/mL,with the correlation coefficients higher than 0.995.the limits of detection(LODs)were found to be 0.05 mg/kg,and the limits of quantification(LOQs)were found to be O.1 mg/kg.The average recoveries of four novel nafil derivatives at three spiked levels of 1,2,and 10 times the limit of quantification in blank matrix were in the range of 80.13~105.97%,with the relative standard deviation between 0.11~7.75%.This method was used to analyze 121 batches of collected samples,and a total of 17 batches of positive samples were detected,with a content range of 27.92~5910 mg/kg.This method is efficient and accurate,and meets the qualitative and quantitative analysis requirements for the illegal addition of four new nafil derivatives in food,effectively filling the regulatory gap for these four new illegal nafil derivatives in food.
作者
吴婉琴
范小龙
夏金涛
朱松松
江丰
王亨
胡玮
冯猛
WU Wan-qin;FAN Xiao-long;XIA Jin-tao;ZHU Song-song;JIANG Feng;WANG Heng;HU Wei;FENG Meng(Hubei Provincial Institute for Food Supervision and Test,Wuhan 430075,China;Key Laboratory of Detection Technology of Focus Chemical Hazards in Animal-derived Food for State Market Regulation,Wuhan 430075,China;Hubei Provincial Engineering and Technology Research Center for Food Quality and Safety Test,Wuhan 430075,China;Hubei Shizhen Laboratory,Wuhan 430065,China;Waters Corporation,Shanghai 201206,China)
出处
《化学研究与应用》
北大核心
2025年第9期2797-2804,共8页
Chemical Research and Application
基金
国家市场监督管理总局科技创新人才计划(青年拔尖人才)项目(QNBJ202330)资助
国家市场监督管理总局科技计划项目(2024MK085)资助
国家市场监督管理总局科技计划项目(2022MK085)资助
国家重点研发计划项目(2023YFF1104704-03)资助。
关键词
液质联用法
新型那非衍生物
食品
非法添加
high-performance liquid chromatography-mass spectrometry(HPLC-MS)
novel nafil derivatives
food,llegal additions
