固相萃取-毛细管柱气相色谱-质谱测定土壤和蔬菜中三唑酮残留量
Capillary Column-GC-MS Determination of Residual Triadimenfon in Soil and Vegetable with Separation by Solid Phase Extraction
摘 要
提出固相萃取分离,毛细管柱气相色谱和质谱联用法测定土壤及蔬菜中三唑酮的残留量.试样用乙腈提取,所得提取液在80 ℃吹氮至近干,并加正己烷2 mL溶解残渣.此溶液流经填充酸性氧化铝的固相萃取小柱,用正己烷-丙酮(2+1)混合溶剂淋洗小柱,使土壤样品中存在的硫磺与需测定的三唑酮分离.用正己烷-丙酮(1+3)混合溶剂将三唑酮从小柱上解吸洗下,所得洗出液蒸发浓缩,用正己烷定容为5.0 mL供GC-MS分析用.测定中用三唑酮标准溶液制备浓度范围在0.006~1.44 mg·L-1之间的标准曲线.方法的检出限(3S/N)为0.001 mg·kg-1.在3个浓度水平上对方法的回收及精密度作了试验,测得其回收率及相对标准偏差(n=5)依次在84%~92%及1.93%~4.04%之间.
固相萃取
酸性氧化铝
硫
三唑酮
土壤
蔬菜
GC-MS
SPE
Acidic aluminum oxide
Sulfur
Triadimenfon
Soil
Vegetable
Abstract
A method of capillary column gas chromatography-MS with separation by SPE was proposed for the determination of triadimenfon in soil and vegetables.Triadimenfon in the sample was extracted with acetonitrile and the extract was evaporated to near dryness by N2-blowing at 80 ℃.The residue was taken up with 2 mL of n-hexane and purified further by passing through a SPE micro-column packed with acidic aluminum oxide and rinsing with a mixed solvent of n-hexane and acetone (2+1) to remove sulfur which is usually existed in soil samples.Triadimenfon on the column was then eluted with n-hexane-acetone (1+3) mixture and the eluate was concentrated and made up to 5.0 mL with n-hexane which was ready for GC-MS analysis under the prescribed conditions.Standard curve was prepared with triadimenfon solution in the concentration range of 0.006-1.44 mg·L-1.Limit of detection (3S/N) of the method was found to be 0.001 mg·kg-1.Results of tests for recovery and precision at 3 concentration levels were found in the ranges of 84%-92% and (RSD) 1.93%-4.04% respectively.
中图分类号 O657.31
所属栏目 工作简报
基金项目 云南省农业科技攻关项目(2006NG01)资助
收稿日期 2007/12/28
修改稿日期
网络出版日期
作者单位点击查看
备注王志飞(1982-),男,山西运城人,硕士研究生,主要从事食品安全研究.
引用该论文: WANG Zhi-fei,LI Qi-wan,WANG Zhen-jun,ZHAO Ji-shou,ER Zhu,LIU Hong-cheng. Capillary Column-GC-MS Determination of Residual Triadimenfon in Soil and Vegetable with Separation by Solid Phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2009, 45(2): 175～177
王志飞,黎其万,王振军,赵吉寿,佴注,刘宏程. 固相萃取-毛细管柱气相色谱-质谱测定土壤和蔬菜中三唑酮残留量[J]. 理化检验－化学分册, 2009, 45(2): 175～177
被引情况:
【1】叶存玲,伍心妮,刘珂珂,王治科, "多壁碳纳米管固相萃取-高效液相色谱法测定水中三唑酮",理化检验－化学分册 49, 1038-1041(2013)
共有人对该论文发表了看法，其中：
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
参考文献
【1】刘毅华,杨仁斌,郭正元.三唑酮在油菜及土壤中的残留动态[J].农药,2004,43(12):559-560．
【2】牛红红,王岩,逯忠斌,等.三唑酮在甘蓝及土壤中的残留动态研究[J].吉林农业大学学报,2005,27(2):209-211．
【3】Tang F,Yue Y,Hua R,et al.Matrix solid-phase dispersion microextraction and determine-ation of pesticide residues in medicinal herbs by gas chromatography with a nitrogen-phosphorus detector[J].J AOAC Int,2006,89(2):498-502．
【4】Singh N.Factors affecting triadimefon degradation in soils[J].J Agric Food Chem,2005,53:70-75．
【5】Runes H B,Jenkins J J,Field J A.Method for the analysis of triadimefon and ethofumesate from dislodgeable foliar residues on turfgrass by solid-phase extraction and in-vial elution[J].J Agric Food Chem,1999,47(8):3252-3256．
【6】Schermerhorn P G,Golden P E,Krynitsky A J,et al.Determination of 22 triazole compounds including parent fungicides and metabolites in apples,peaches,flour,and water by liquid chromatography/tandem mass spectrometry[J].J AOAC Int,2005,88(5):1491-1502．
【7】Wu Y S,Lee H K,Li S F.High-performance chiral separation of fourteen triazole fungicides by sulfated beta-cyclodextrin-mediated capillary electrophoresis[J].J Chromatogr A,2001,912(1):171-179．(上接第174页)Bias J D,Mateos N R,Sanchez A G.Detennination of total As and Se in soils and plants by FIA-AAS-HG analysis coupled techniques[J].Journal of AOAC International,1996,79(3):764-768．
【8】汤毅珊.微波消解-原子荧光法测定中药中的汞、砷[J].中药新药与临床药理,1999,11(3):177-179．
【9】国家环保总局.水和废水监测分析法指南(下册)[M].北京:中国环境科学出版社,1994．
【2】牛红红,王岩,逯忠斌,等.三唑酮在甘蓝及土壤中的残留动态研究[J].吉林农业大学学报,2005,27(2):209-211．
【3】Tang F,Yue Y,Hua R,et al.Matrix solid-phase dispersion microextraction and determine-ation of pesticide residues in medicinal herbs by gas chromatography with a nitrogen-phosphorus detector[J].J AOAC Int,2006,89(2):498-502．
【4】Singh N.Factors affecting triadimefon degradation in soils[J].J Agric Food Chem,2005,53:70-75．
【5】Runes H B,Jenkins J J,Field J A.Method for the analysis of triadimefon and ethofumesate from dislodgeable foliar residues on turfgrass by solid-phase extraction and in-vial elution[J].J Agric Food Chem,1999,47(8):3252-3256．
【6】Schermerhorn P G,Golden P E,Krynitsky A J,et al.Determination of 22 triazole compounds including parent fungicides and metabolites in apples,peaches,flour,and water by liquid chromatography/tandem mass spectrometry[J].J AOAC Int,2005,88(5):1491-1502．
【7】Wu Y S,Lee H K,Li S F.High-performance chiral separation of fourteen triazole fungicides by sulfated beta-cyclodextrin-mediated capillary electrophoresis[J].J Chromatogr A,2001,912(1):171-179．(上接第174页)Bias J D,Mateos N R,Sanchez A G.Detennination of total As and Se in soils and plants by FIA-AAS-HG analysis coupled techniques[J].Journal of AOAC International,1996,79(3):764-768．
【8】汤毅珊.微波消解-原子荧光法测定中药中的汞、砷[J].中药新药与临床药理,1999,11(3):177-179．
【9】国家环保总局.水和废水监测分析法指南(下册)[M].北京:中国环境科学出版社,1994．
相关信息
