高效液相色谱-串联质谱测定奶粉中3种苯并咪唑类药物残留  

Determination of Three Benzimidazole Residues in Milk Powder Using HPLC-MS/MS

作　　者：汤娟[1] 吴斌[2] 景苏[1] 蒋原[2] 陈惠兰[2] 丁涛[2] 沈崇钰[2] 

机构地区：[1]南京工业大学理学院,江苏南京210009 [2]江苏出入境检验检疫局动植物与食品检测中心,江苏南京210001

出　　处：《质谱学报》2012年第1期13-17,共5页Journal of Chinese Mass Spectrometry Society

基　　金：科技部质检公益项目(养殖与屠宰环境中污染物检测技术研究No.200810099)资助

摘　　要：建立了高效液相色谱-串联质谱测定全脂和脱脂奶粉中奥芬达唑,阿苯达唑和芬苯达唑3种苯并咪唑类杀虫剂残留的方法。通过比较不同溶液的提取效率,最终选择含1%乙酸的甲醇作为提取溶液,正己烷和阳离子固相萃取两步净化,有效去除奶粉基质中的抑制干扰物。以乙腈和含0.5mmol/L醋酸铵及0.1%甲酸的水溶液为流动相,C18作为分析色谱柱,采用梯度洗脱方式进行液相色谱分离。脱脂奶粉和全脂奶粉3个添加水平的回收率范围为70.0%～85.8%,相对标准偏差均小于7.5%,在2～100μg/L浓度范围内,线性相关系数大于0.997 3,方法检测限为10μg/kg,能满足现有各国残留限量要求。A method for simultaneous determination of oxfendazole,albendazole and fenbendazole residues in milk powder was developed by high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）.By comparison the extraction effect of different solutions,1% acetic acid-methanol was finally selected as the extracting solution.Two consecutive steps of N-hexane and cationic solid phase extraction were used to remove the interferences in milk powder.Gradient elution programme was performed on a C18 column using a mobile phase consisting of acetonitrile and 0.5 mmol/L ammonium acetate-0.1% formic acid solution.Recoveries of skim milk and whole milk powder are in the range of 70.0%—85.8%.The conrrelation coefficient is greater than 0.997 3 in the 2—100 μg/L.The method detection limit is 10 μg/kg,and it can be meet all the requirements of national residues level.

关 键 词：高效液相色谱-串联质谱 奥芬达唑 阿苯达唑 芬苯达唑 奶粉 

分 类 号：O657.63[理学—分析化学]