气相色谱法同时测定禾谷类农作物中甲草胺、乙草胺和丁草胺
曲颖超,王岩,王盛男,李雯雯,索力墨
赤峰市农牧科学研究院,农业面源污染研究中心,内蒙古赤峰 024031
Simultaneous determination of alachlor, acetochlor and butachlor in cereal crop by gas chromatography
QU Yingchao, WANG Yan, WANG Shengnan, LI Wenwen, SUO Limo
Chifeng Institute of Agriculture and Animal Husbandry, Inner Mongolia, Chifeng 024031, China
摘要:建立气相色谱法同时测定禾谷类农作物中甲草胺、乙草胺和丁草胺3种酰胺类除草剂的分析方法。谷物样品用乙腈、氯化钠超声提取,用弗罗里矽硅土固相萃取柱净化,提取液经0.22 μm有机滤膜过滤,以气相色谱(ECD检测器)检测。结果表明,甲草胺、乙草胺和丁草胺的质量浓度在0.1~2.0 mg/L范围内与色谱峰面积呈良好的线性关系,相关系数分别为0.999 8,0.999 8和0.999 6,检出限分别为0.001 8,0.001 7和0.001 3 mg/kg,定量限分别为0.005 5,0.005 1和0.004 0 mg/kg。在加标水平为0.4,2.0和3.6 mg/kg时,3种酰胺类除草剂的平均回收率为90.7%~104.8%,相对标准偏差为0.61%~3.97%(n=6)。该方法准确,灵敏,操作简单,适用于禾谷类农作物中甲草胺、乙草胺和丁草胺残留量的同时测定。
Abstract:A method for simultaneous determination of alachlor, acetochlor and butachlor in cereal crops by gas chromatography was established. The cereal samples were extracted by ultrasonic with acetonitrile and sodium chloride, and purified with florisil solid phase extraction column. The extracts were filtered with 0.22 μm organic membrane, and detected by gas chromatography(ECD detector). The results showed that the mass concentration of alachlor, acetochlor and butachlor had a good linear relationship with the chromatographic peak area in the range of 0.1-2.0 mg/L, and the correlation coefficients were 0.999 8, 0.999 8, 0.999 6, respectively. The the detection limits of alachlor, acetochlor and butachlor were 0.001 8, 0.001 7 and 0.001 3 mg/kg, and the quantitation limits were 0.005 5, 0.005 1 and 0.004 0 mg/kg, respectively. When the spiked levels were 0.4, 2.0 and 3.6 mg/kg, the average recoveries of the three amide herbicedes were 90.7%-104.8%, and the relative standard deviations were 0.61%-3.97%(n=6). The method is accurate, sensitive, simple which is suitable for the simultaneous determination of the alachlor, acetochlor and butachlor residues in cereal crops.
关键词:气相色谱法;禾谷类农作物;甲草胺;乙草胺;丁草胺
Keywords:gas chromatography; cereal crop; alachlor; acetochlor; butachlor
基金:农业基础长期性科技工作,国家农业环境数据中心和国家土壤质量数据中心观测监测任务(ZX03S0509,ZX02S050900);赤峰市玉龙人才工程项目
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曲颖超,王岩,王盛男,等.气相色谱法同时测定禾谷类农作物中甲草胺、乙草胺和丁草胺[J].化学分析计量,2020,29(6):23-27.
QU Y C,WANG Y,WANG S N,et al. Simultaneous determination of alachlor,acetochlor and butachlor in cereal crop by gas chromatography[J]. Chemical analysis and meterage,2020,29(6):23-27.
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