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固相萃取-柱前衍生-气相色谱-质谱联用法测定水中2,4-滴和灭草松 被引量:25

GC-MS Determination of 2,4-D and Bentazone in Water with Pretreatment by SPE and Pre-column Derivatization
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摘要 水样中两种除草剂,2,4-滴及灭草松,用SPE法经Oasis HLB柱分离富集。用甲醇及甲基叔丁基醚(10+90)混合溶剂作洗提液将此两种除草剂从SPE小柱上洗脱,所得洗脱液经吹氮蒸干和用碘甲烷-二氯甲烷溶液及四丁基硫酸氢铵氢氧化钠溶液进行柱前衍生化,所得衍生物经干燥后溶于正己烷1.0mL中,所得溶液供GC-MS测定,所测得的峰面积值与2,4-滴或灭草松的浓度在0.1~5.0mg·L^-1范围内呈线性关系。当用200mL水样进行分析时测得此方法的测定下限(10S/N)依次为0.02μg·L^-1及0.10μg·L^-1。 Two herbicidal chemicals, 2,4-D (dichloro-phenoxy acetic acid) and bentazone in water samples were separated and enriched by SPE on Oasis HLB SPE micro-column. Mixed solvent of CH3 OH and methyl-tert. butyl ether (10+90) was used to elute the 2 herbicidal chemicals from the column and the eluate was dried by N2- blowing, made up to 1.0 mL with hexane and used for GC-MS determination after pre-column derivatization with iodomethane-dichloromethane (10 + 90) solution and tetra-butyl-ammonium hydrogen sulfate-NaOH solution. Linear relationship between values of peak area and concentration of either 2,4-D or bentazone was obtained in the range of 0. 1-5. 0 mg·L^-1. Values of lower limit of determination (10S/N) found were 0. 02μg·L^-1 for 2,4-D and 0. 10 μg·L^-1 for hentazone when 200 mL of water samples were introduced.
作者 彭敏 刘传生
出处 《理化检验(化学分册)》 CAS CSCD 北大核心 2009年第7期791-793,共3页 Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
关键词 气相色谱-质谱联用法 2 4-滴 灭草松 水样 GC-MS 2,4-D Bentazone Water sample
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