摘要
本研究建立了超高效液相色谱-串联质谱法测定鲜乳中异丙噻菌胺和联苯吡菌胺的分析方法,考察了不同实验条件对鲜牛乳中异丙噻菌胺和联苯吡菌胺的提取效果。以乙腈为提取溶剂,经超声提取、冷冻离心分层,采用C_(18)色谱柱分离,0.2%甲酸水和乙腈作为流动相梯度洗脱,在正离子扫描模式下采用电喷雾电离多反应监测模式进行测定,基质匹配曲线,外标法定量。结果异丙噻菌胺和联苯吡菌胺在0.1~10.0μg/L质量浓度范围线性良好,相关系数(R^(2))分别为0.9991和0.9993,方法检出限(LODs)分别为0.2μg/kg和0.4μg/kg,定量限(LOQs)均为1.2μg/kg。结果表明,该方法灵敏度高,定量限低,操作简便,成本较低,可满足鲜牛乳中异丙噻菌胺和联苯吡菌胺的定量检测要求。
In this study,an analysis method for determination of isofetamid and bixafen compounds in raw milk by ultra high performance liquid chromatography-tandem mass spectrometry.The extraction of isofetamid and bixafen in raw milk under different experimental conditions was investigated.Acetonitrile was used as the extraction solvent.C_(18)column was used for separation,after ultrasound extraction and refrigeration centrifugation stratification.0.2%formic acid water and acetonitrile were used as mobile phase for gradient elute,and the electrospray ionization multiple reaction monitoring mode(MRM)was used in positive ion scanning mode,then the matrix standard curve was used to quantitative analysis by external standard.Good linearity in range of 0.1-10.0μg/L were observed for Isofetamid and bixafen,the correlation coefficient(R^(2))were 0.9991 and 0.9993,respectively.The limits of detection(LODs)were 0.2μg/kg and 0.4μg/kg,the limits of quantitative(LOQs)both were 1.2μg/kg.It was concluded that the method has high sensitivity,low LOQs,convenient operation and low cost,which can meet the quantitative detection requirements for isofetamid and bixafen in raw milk products.
作者
鲁琰农
逯刚
许博舟
聂雪梅
谢昀
董立雅
许秀丽
LU Yannong;LU Gang;XU Bozhou;NIE Xuemei;XIE Yun;DONG Liya;XU Xiuli(Institute of Food Safety,Chinese Academy of Inspection and Quarantine,Beijing,100176,China;Inner Mongolia Meng-Niu Dairy(Group)Co.,Ltd.;Gansu Food Inspection and Research Institute;Key Laboratory of Food Quality and Safety for State Market Regulation)
出处
《质量安全与检验检测》
2023年第2期1-5,41,共6页
QUALITY SAFETY INSPECTION AND TESTING
