摘要
建立了玉米籽粒中三嗪类除草剂及其代谢物残留的气相色谱化学电离二级质谱(GC-CIMS/MS)分析方法。样品采用盐酸和乙腈混合溶液均质提取,石墨化碳黑(GCB)与中性氧化铝的混合固相萃取柱净化,GC-CIMS/MS基质外标法测定。三嗪类除草剂及代谢物在0.05(0.10)～4.0mg/L范围内线性良好,相关系数r在0.9939以上(脱乙基莠去津溶剂标准曲线的r=0.9894);在0.050、0.100μg/g添加水平,平均添加回收率为72%～108%,相对标准偏差为3.09%～20.14%,满足进出口及残留监控测定的需要。
A gas chromatography chemical ionization tandem mass spectrometry （ GC - CI MS/MS） method was established for simultaneous determination of triazine herbicides and some metabolites res- idues in maize. The sample was extracted by homogenization using a mixed solution consisted of aceto- nitrile and hydrochloric acid. The extract were cleaned up by graphite carbon black （GCB） and neu- tral-A1203 mixed solid phase extraction column. The target compounds were analyzed by GC - CI MS/ MS and quantified by an external standard method. The linear ranges of seven compounds were 0.05 - 4. 0 mg/L for solvent matrix and 0. 1 - 4.0 mg/L for maize matrix, respectively. All the correla- tion coefficients were above 0. 993 9 （ except the solvent standard curve of desethyl atrazine, r = 0. 989 4）. The average recoveries of seven compounds from maize samples at two fortification levels of 0. 050 and O. 100 μ/g ranged from 72% to 108% , and the relative standard deviations（RSDs） were in the range of 3.09% - 20. 14%. All the limits of detection（LODs） were lower than 0.05μg/g. The method was inexpensive and effective, and could meet the requirement on the import ＆ export inspection monitoring for simultaneous determination of triazine herbicides and some metabolites in maize.
出处
《分析测试学报》
CAS
CSCD
北大核心
2009年第1期96-100,共5页
Journal of Instrumental Analysis
