凝胶渗透色谱-高效液相色谱-串联质谱法测定花生油中涕灭威及其代谢.docVIP

凝胶渗透色谱-高效液相色谱-串联质谱法测定花生油中涕灭威及其代谢产物残留量 吉文亮 刘华良 马永建 江苏省疾病预防控制中心， 南京 210009 《卫生研究》2001年39卷04期 摘要：目的 测定花生油中涕灭威及其代谢产物涕灭威亚砜和涕灭威砜残留量。方法 花生油样品加入同位素内标d3-涕灭威后经凝胶渗透色谱净化和在线浓缩，以甲醇-10mmol/L乙酸铵溶液为流动相，经HPLC梯度分离后质谱以多反应监测模式（MRM）测定。结果 涕灭威亚砜和涕灭威砜的[M+H]+离子响应最强作为母离子,而涕灭威以[M+NH4]+作为母离子。涕灭威及其代谢产物的工作曲线线性范围为5~250ng/mL，相关系数均优于0.998（r2），涕灭威及涕灭威砜的检出限为2.0μg/kg，涕灭威亚砜的检出限为1.0μg/kg，在加标浓度分别为10μg/kg 和100μg/kg时的回收率为85.2％～117.4%，相对标准偏差为7.59%～11.0%。结论 建立的方法快捷、灵敏度高，可应用于同时测定花生油中农药涕灭威及其代谢物涕灭威亚砜、涕灭威砜的残留量。 关键词：凝胶渗透色谱 高效液相色谱-串联质谱 涕灭威 涕灭威亚砜 涕灭威砜 同位素内标 花生油 Determination of aldicarb and its metabolites in peanut oil using Gel permeation chromatography –high performance liquid chromatography –tandem mass spectrometry JI Wenliang, LIU Hualiang ,MA Yongjian Jiangsu Provincial Center for Disease Control and Prevention ，Nanjing 210009，China Abstract: Objective To determinate aldicarb and its metabolites aldicarb sulfoxide and aldicarb sulfone in peanut oil. Methods Peanut oil was purified with GPC and concentrated online after adding isotopically labeled standards as internal standards. The mobile phase composed with methanol and 10mmol/L ammonium acetate. Data acquisition was achieved by applying multiple reaction monitoring of two fragment ion transitions to provide a high sensitivity and selectivity for both quantification and confirmation. Resluts. Strong signals corresponding to [M+H]+ were observed for aldicarb sulfoxide and aldicarb sulfone as parent ions, except [M+NH4]+ for aldicarb in optimized procedure. The matrix-matched calibration curves showed good linearity in the range 5~250ng/mL with correlation coefficients larger than 0.998(r2). The limits of detection were 2.0μg/kg for aldicarb and aldicarb sulfone, 1.0μg/kg for aldicarb sulfoxide. The recoveries were ranged from 85.2％ to 117.4% with the relative standard deviation ranged from 7.59% to 11.0% when spiked levels at 10μg/kg and 100μg/kg. Conclusion The method was sensitive and selective for determination of aldicarb and its metab