气相色谱法同时测定大豆中13种苯氧羧酸类除草剂的残留量
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R15 O657.71[著者标引]

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国家食品安全专项基金


Simultaneous Determination of Multiple Phenoxy Acid Herbicide Residues in Soybean by Gas Chromatography
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    摘要:

    为检测大豆中的苯氧羧酸类除草剂残留,建立了大豆中13种苯氧羧酸类除草剂(对氯苯氧乙酸、对氯苯氧丙酸、苯氧丁酸、麦草畏、2甲4氯苯氧乙酸、2甲4氯苯氧丙酸、2甲4氯苯氧丁酸、2,4-滴、3,4-滴、2,4,5-涕、2,4,5-涕丙酸、2,4-滴丙酸、2,4-滴丁酸)多残留量的气相色谱检测方法。样品经过正己烷预除脂后用乙腈和50mmol/L盐酸混和液(体积比7 3)提取,提取液经过与乙腈饱和的正己烷液液分配除脂,阴离子交换柱净化后用五氟溴苄衍生化。衍生产物经硅胶柱净化后,采用气相色谱(GC)-电子捕获检测器(ECD)检测,外标法定量。13种苯氧羧酸类除草剂在质量浓度0.005~0.1mg/kg之间,与峰面积呈线性关系,相关系数为0.9954~0.9993;0.01和0.1mg/kg2个水平的加标回收率均在70%以上,相对标准偏差小于20%,方法的检测限(S/N≥3)满足主要贸易国最大残留限量要求。

    Abstract:

    A technique for simultaneous determination of 13 phenoxy acid herbicide residues in soybean was developed.Phenoxy acid herbicides were extracted with acetonitrile-50 mmol/L HCl(volume ratio was 7 3),followed by liquid-liquid partition with n-hexane.The soybean extract was further cleaned up by anion exchange column and derivatized with pentafluorobenzyl bromide.The resulting esters were determined by gas chromatography equipped with electron capture detector.The pre-treatment method was critically examined.Recoveries of two fortified levels(0.01 and 0.1 mg/kg)were above 70%.and the coefficients of variation were less than 20%.It showed that this method can meet the requirements of multi-residue analysis in the inspection of import/export soybean commodities.

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匡华,储晓刚,侯玉霞,祁彦.气相色谱法同时测定大豆中13种苯氧羧酸类除草剂的残留量[J].中国食品卫生杂志,2006,(6).

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