1HNMR法定量测定土壤中除草剂2,4-二氯苯氧乙酸
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国家自然科学基金项目(31071702)和广东省自然科学基金项目(8151064201000029)


Quantitative detection of 2,4-dichlorophenoxyacetic acid residue in soil using 1HNMR
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    摘要:

    建立了一种用内标法快速、简便检测土壤中2,4-二氯苯氧乙酸(2,4-dichlorophenoxyacetic acid,2,4-D)的1HNMR分析方法。土壤中样品经pH值2.0的酸性水溶液和丙酮提取、浓缩、定容,用布鲁克AV 600 核磁共振仪检测;在25 ℃下,以甲醇为溶剂、内置氘代丙酮为锁场溶剂,均苯三甲酸为内标,观察频率在600.13 MHz,谱宽为9 001.95 Hz,90°脉冲宽度12.10 μs,采集时间3 s,延迟时间3 s,累加次数128的条件下采集2,4-D试样的氢谱。线性范围为 30.00~200.00 mg/L,最低检测限25.0 mg/kg。稻田土和果园土的平均添加回收率分别为83.54%~90.26%和85.26%~92.65%,变异系数分别为为3.82%~5.15%和2.32%~5.89%。

    Abstract:

    An 1HNMR method for quantitative detecting 2,4-dichlorophenoxyacetic acid in soil with 1,3,5-benzenetricarboxylic acid(BTC) as internal standard was developed.Proton nuclear magnetic resonance spectroscopy (1HNMR) spectra were obtained in methanol and acetone-d6 with a Bruker AV 600 MHz spectrometer at 25 ℃.For each sample,128 scans were recorded with the following parameters:observing frequency (600.13 MHz),spectra width (9 001.95 Hz),90° pulses width (12.10 μs) ,acquisition time (3 s) and delay time (3 s).The linearity range is 30.00-200.00 mg/L,the minimum detection of 2,4-D was 25.0 mg/kg.The average recoveries of 2,4-D in paddy soil and garden soil were 83.54%-90.26% and 85.26%-92.65% with CVs of 3.82%-5.15% and 2.32%-5.89%,respectively.

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杨晓云,毛秋平,黄其亮,徐汉虹.1HNMR法定量测定土壤中除草剂2,4-二氯苯氧乙酸[J].华中农业大学学报,2011,30(3):348-351

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  • 收稿日期:2010-12-04
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