摘要
建立了高效液相色谱质谱联用检测牛奶中阿特拉津及其两类代谢物残留的同步分析方法。样品中加入1%HCl和0.265 mol/L Na2S2O3后,由冰乙腈提取,混合型阳离子交换柱固相萃取净化,采用液相色谱-串联质谱进行测定,外标法定量。阿特拉津及其代谢物在0.4～100μg/L范围内线性良好,标准曲线相关系数R2>0.99。在1～25μg/L浓度范围内,除脱异丙基羟基阿特拉津的平均加标回收率较低约为64.2%外,其它目标物的回收率在75.0%～119.0%之间,相对标准偏差为1.5%～14.5%;脱乙基阿特拉津、羟基阿特拉津、脱乙基羟基阿特拉津的检出限为0.1μg/L;其余目标物的检出限为0.5μg/L。本方法的灵敏度较高,且简便、快速,可以较好地解决目标物极性差别大及样品基质对检测结果的干扰等问题,可以满足牛奶中阿特拉津及其两类代谢物残留检测的需要。
A sensitive LC-MS method was developed for the determination of atrazine and its metabolites in cattle milk. The method can be applied to the simultaneous determination of atrazine and its major dealkylation and hydroxylation metabolites which include atrazine, hydroxyatrazine, diaminochloroatrazine, desisopropylatrazine, desethylatrazine, deethylhydroxyatrazine, deisopropylhydroxyatrazine. The analytical scheme including sample preparation, chromatographic and mass spectrometric conditions was developed and optimized. Hydrochloric acid and sodium thiosulphate were added to the sample before extracted by ice aeetonitrile. The mixed cation-exchange column was found to be satisfactory for the purification of sample. High-performance liquid chromatography/mass spectrometric methods were used for the quantitative analysis of samples. The relative standard deviations for the analytes were from 1.53% to 9.04% at 1, 5, I0 and 25 μg/L level, the recoveries range was from 62.0% to 119.0% at 1, 5, 10 and 25 μg/L level, and the limits of detection （LOD） were from 0.1 to 0.5 μg/L. The linear ranges of the method were from 0.4 to 100 μg/L with R2 values of greater than 0.99. The method is rapid, cost-effective and could be applied to assess the safety of milk exposure to atrazine related chemicals.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2013年第1期128-132,共5页
Chinese Journal of Analytical Chemistry
关键词
液相色谱质谱联用
牛奶
阿特拉津
代谢物
Liquid chromatography-tandem mass spectrometry
Milk
Atrazine
Metabolites
